Document 3e8VVLBoX2k5pz1Dpqa97dL8x

U.S. PEP`riMflJT Of KEimii. EOBP'T! A If LFAffE F. j i:L Cr2 /Miniflisiratioi! VOLUME 6 No. 6, Consecutive N>. 36 may 1970 Helen L. Reynolds, Editor Nancy J. Palmer, Laura A. Kovach, and Alberta E. Blair, Assistants Dorothy H. Mahoney and Joanne A.ltken, Page Makeup IN THIS ISSUE Collaborative Study of the Determination of Ammonia as an Index of Decomposition in Crabmeat by Kurt Steinbrecher........................... 281 Spectrofluorometric Determination of Ra:.vc1f1a Serpentina Tablets and Whole Root by Charles C. Crark......................................... 288 Application of Neutron Activation Analytes to Food Products*. A Bibliography by James T. 'fanner and Melvin Friedman.................. 294 Polarographic Determination of Nitrates in Aqueous Media Containing Nitrites by Albert L. Woodson .............................................. 299 Correlation of Organoleptic Evidence with pH, Volatile Bases, and Indole as Indices of Decomposition in Raw, Frozen Shrimp by Billy G. Miles............................................................................. .... 304 Differential Effects of DDT and Polychlorinated Biphenyls on the Central Nervous System by Thomas J. Sobotka................................ 313 Microbiological Contamination Bibliography (Continued) by Harriet M. Oxley.................................................................................................... 320 Publications List......................................... ............................................................... 325 Cumulative Index to Interbureau By-Lines, Vols. 1-6............................328 ! DSW 033449 STLCOPCB4017411 Interbureau By-Lines No. 6 May 1970 COLLABORATIVE STUDY OF THE DETERMINATION OF AMMONIA AS AN INDEX OF DECOMPOSITION IN CRABMEAT Kurt Steinbrecher, Seattle District The study by Burnett (1) showed that a general correlation existed between the concentration of ammonia in crabmeat and its degree of decomposition by organoleptic standards. The method is based on the color formation observed after the reaction of ammonia, thymol, and alkaline bromine water. The reaction scheme may be suggested to be analogous to the indophenol mechanism proposed by Bolleter jet al. (2): 281 * DSW 033450 ... .1. LU. STLCOPCB4017412 282 V Fernandez-Flores and Salwin (3) modified the method, applied it to cod fish, and noted an 8-fold increase in sensitivity. With some slight modification this method was adapted to crabmeat and col.laboratively studied. Collaborative Study Eleven collaborators representing 7 Food and Drug laboratories, 2 Bureau of Commercial Fisheries laboratories, and 1 university laboratory participated in the study. The samples were prepared in the following manner: Fresh frozen Dungencss crab was allowed to thaw in the shell at room temperature. It was sampled organoleptically from time to time, and meat at a particular stage of decomposition was removed from the shell, ground 3 times through a meat grinder with thorough mixing, and frozen for subsequentdistribution to collaborators. Collaborators were requested to analyze 6 samples: I. Early Class 1. II. Late Class 1. III. Borderline Classes 1 and 2. ' J) IV. Middle Class 2. V. Middle Class 3. . ' VI. Middle Class 3. The definition of the classes conforms to the usage of Hillig et al.. (4). METHOD (Use NH3 - free water throughout; ordinary distilled water is suitable.) Reagents (a) Bromine solution.--Dissolve 1.0 ml bromine in 100 ml 0.4]S[ NaOH (solution is stable 3 days in dark bottle). (b) Thymol solution.--10% w/v in ethyl alcohol (solution is stable 3 days In dark bottle). 0 DSW 033451 STLCOPCB4017413 283 (c) Ammonia standard solution.--Dissolve 0.314 g NH^Cl, previously dried 1 hr at 100C, in water and dilute to 100 ml. Transfer 1.0 ml to 100 ml volumetric flask and dilute with water (10 p.g NH-j/ml), (d) n-Butyl alcohol. (e) -3N NaOH. (f) Phosphotungstic acid.--2.5% w/v aqueous solution. Procedure Place 20 g prepared sample in 500 ml conical glass-stoppered flask. Add 180 ml phosphotungstic acid solution. Shake vigorously 2 min and filter through paper (Whatman No. 1, or equivalent), collecting filtrate in 250 ml glass-stoppered conical flask, Pipet 1.0 ml filtrate (representing 0.1 g crabmeat) into.50 ml glass-stoppered conical flask. Save remainder of filtrate. Add. 1.0 ml phosphotungstic acid solution to separate flask for blank. To each flask add 9.0 ml water*, then add 2.0 ml thymol solution and 5.0 ml bromine solution in that order, mixing thoroughly after each addition. . Let stand 10-15 min. Add 1.0 ml 3N^ NaOH, mix, and let stand at lea?t 20 min. . Transfer each solution to separate 125 ml separatory funnel. Rinse flasks with 10 ml water, adding rinse to proper funnel. Add 30.0 ml n-butyl alcohol and shake vigorously. Discard lower aqueous phase and drain alcohol into glass-stoppered conical flask through glass funnel plugged with glass wool and containing ca 45 g anhydrous sodium sulfate. Measure absorbance of solution at 682 nm in 1 cm cell with blank in reference cell. Standard Preparation Transfer 0, 1.0, 2.0, 3.0, 4.0, 5.0, 6.0, and 7.0 ml standard ammonia solution to separate 50 ml glass-stoppered conical flasks. Add 1.0 ml phosphotungstic acid solution to each flask. Dilute contents in each flask to 10 ml with water and proceed with prepara tion of standard solution as in procedure, beginning with "then add 2.0 ml thymol solution...". Using portion of 0 standard as blank, measure absorbance of all 8 standard solutions at 682 nm in 1 cm cell against blank in reference cell. *lf final absorbance reading is > 1.0 absorbance unit, dilute filtrate with phosphotungstic acid solution so that 1.0 ml dilute solution will produce an absorbance reading below this level. DSW 033452 JT STLCOPCB4017414 Results and Discussion To minimize errors resulting from reading concentrations from a graphic representation of the standard curve, we decided to derive the equation of the standard curve by the least squares method and to obtain the concentration values by substituting sample absorbances in the equation derived. To reduce calculation errors, collaborators were asked to report absorbance values only for the standards and absorbance values and dilutions performed for the samples. All calculations converting absorbance values to pg Nl^/g crabmeat were performed by the Associate Referee. It Boon became; apparent that we would need to be cautious about evaluating the results and drawing conclusions. A majority of the collaborators in some way did not follow the instructions. In several cases the method was modified; in others several runs were reported so that the Associate Referee had to select the data to be used in the study. Nevertheless, each set of results was carefully scrutinized and a series of values from each collaborator was selected that was thought to be representative of the method as it was intended to be performed. Table 1 listg the amount of ammonia found in the crabmeat samples in pg Nir^/g crabmeat. On the basis of the two-tailed ranking test for 11 laboratories and 6 materials (5), results from Collaborator 8 were eliminated from further calculations. The means with their standard deviations for the remaining samples are shown in Table 2. Certain preliminary conclusions may be drawn from the data obtained in this study. There appears to be a direct relationship between the amount of ammonia present in crabmeat and its stage of decomposition, according to organoleptic criteria. However, the results do not present as sharp demarcations between classes of decompositon as might be desired. It can be seen by examining the data for the ammonia content (Table 2) that values for Early Class 1 and Late Class 1 overlap; in fact, the mean value for Late Class 1 is leas than that of Early Class 1, though the standard deviation for Early Class 1 is greater, indicating a greater scatter of those values. Borderline Classes 1 and 2 also overlap in many cases with Early and Late Class 1, though the average is somewhat higher. On the basis of mean values, there seems to be a better spread between the value of ammonia in the samples in Middle Class 2 and those in Borderline Classes 1 and 2, and also between the values of Middle Class 2 and Middle Class 3. ' 0A DSW 033453 r- *' STLCOPCB4017415 Table 1. Collaborative results of ammonia content in 6 samples, H3 NH^/g crabmeat Coll. Ear.lv Cla .V t 1 2 3 4 5 6 7 > 8* 9 10 11 37 3 485 303 234 320 249 265 634 413 259 370 Late Class 1 Borderline Classes 1-2 342 300 286 234 306 316 299 380 363. 256 .. 198 389 604 449 346 566 277 367 742 581 347 334 Middle Class 2 1311 513 756 1271 1174 502 695 2278 1237 906 1330 Middle Middle Class 3 Class 3 2012 1730 1853 1185 1268 1197 1877 2521 2684 1860 2470 1972 1665 1800 1862 668 1128 . 3185 3385 2819 1692 2390 a "These1 results: eliminated from further calculations. Table 3 lists the ranges of values obtained i one standard deviation (68% of the population) and two standard deviations (95% of the population) of the mean. It can be seen for example, that selecting the value 600 pg Nl^/g crabraeat as the dividing line between definite decomposition (Class 2) and undecomposed meat (Class 1) would yield useful results in 68% of the cases, since no undecomposed samples have values higher than 543 and no decomposed samples have values lower than 636. The more realistic 95% criterion, however, shows overlap, with some undecomposed meat classed as decomposed and some decomposed classed as undecomposed. If a limiting value were set at approxi mately 800 pg KH^/g crabmeat, it would not include all decomposed samples, but no good or borderline samples would be rejected. Most collaborators found some difficulty reproducing the standard curve. The actual values of the absorbances of duplicates varied, as well as the slopes, both on repetition by the same investigator and by comparison with other investigators. Variation in replicate sample DSW 033454 STLCOPCB4017416 286 Table 2. Ammonia content of crabmeat according to its stage of decomposition Class Early Class 1 (n-10) Late Class 1 (n-10) Borderline Classes 1-2 (n-10) Middle Class 2 (n-10) Middle Class 3 (n-20) Mean, Hg NH3/g 328 290 426 970 1866 Std Dev. 82 49 117 334 621 Table 3. Range of ammonia content of crabmeat according to its stage of decomposition Class Mean, ^g NHl/fc 1 Std Dev. 2 Std1 Dev. Early Class 1 Late Class 1 ' Borderline.Classes 1 and 2 Middle Class 2 Middle Class 3 246 410 241 339 309 543 636 1304 1245 + 2487 164 492 192 388 192 + 660 302 1638 624 3108 1 i *nvtm :fg'^rv^wimwmw,i|jii i hi DSW 033455 :::rg` sjrr. STLCOPCB4017417 287 color formation paralleled that of the standard solutions. Such variation seems to account for the relatively large standard deviations of the ammonia content values and hence for the limitation of usefulness of the method, as it stands, in assigning the state of decomposition to the sample. This defect was not apparent to the Associate Referee in his preliminary investigation where relatively good reproducibility on repeated analyses had been obtained. More work is needed to indicate the cause for the variation in color formation. For example, the bromine solution must be definitely alkaline for consistent color development to take place. Further modifications of conditions - reagents, concentrations, manipulations must be studied to assure greater reproducibility of results. Recommendations It is recommended that further work on details of the method be undertaken, and that with the achievement of greater reproducibility and precision an additional collaborative study be initiated. Acknowledgments The Associate Referee wishes to thank the following collaborators: J. N. Gaffke, Jr., Seafoods Laboratory, Oregon State University, Astoria, Ore.; J. Spinelli, Bureau of Commercial Fisheries, Seattle, Wash.; M. H. Thompson, Bureau of Commercial Fisheries, Pascagoula, Miss.; and the following members of the Food and Drug Administration: T. S. Smith, Baltimore; W. A. Hallam, Boston; B. L. McGill, Dallas; R. M. Hoss, Kansas; B. G. Miles, New Orleans; A. Weber, New York; D. L. Andersen and S. E. Artoe, Seattle. . References . (1) Burnett, J. L., ,J* Ass. Off. Anal. Chem. 48, 624-627 (1965), (2) Bolleter, W. T., BuBhman, C. J., and Tidwell, P. W., Anal. Chem. 33, 592-594 (1961). -------- -------- (3) Fernandez-Flores, E., and Salwin, H., J. Ass. Off. Anal. Chem. 51. 1109-1110 (1968). . -------- "" (4) Hilllg, F., Shelton, L. R., Jr., Loughrey, J. H., and Eisner, J., J. Ass. Off. Anal. Chem. 41, 763-764 (1958). (5) Youden, W. J., Statistical Techniques for Collaborative Tests. AOAC, Washington, D.C., 1967, pp. 27-29^ : ' This report of the Associate Referee was presented at the 83rd * Annual Meeting of the AOAC, Oct. 13-16, 1969, at Washington, D. C. DSU 033456 f ................... -U ST STLCOPCB4017418 Interburcau By-Lines No. 6 Hay 1970 SPECTROFLUOROMETR1C DETERMINATION OF RAUWOLFIA SERPENTINA TABLETS AND WHOLE ROOT A/ Charles C. Clark, Baltimore District Rauwolfia serpentina, the powdered root obtained from the plant of the s<.me name, is employed as a hypotensive. An assay- has been developed in this laboratory for Rauwolfla serpentina in both ground whole root and dosage forms. It combines modern extraction techniques with the sensitivity of fluorescence. Identical assays are provided for both the raw material and the dosage forms in the NF XII and the 10th edition of Official Methods of Analysis of the AOAC. The method is capable of yielding con sistent and reliable data if large amounts of highly colored tablet excipients are not present. However, the method is time-consuming, ' occupying a working.day in excess of 8 hr, and uses a 4 hr Soxhlet extraction,' 30 shakeouts, a solvent evaporation step, and a 20 min derivative-formation time in a heated water bath. An amount of sample equivalent to 50 tablets is frequently needed for a single assay. Sample blank absorbance values frequently account for 30% or more of the total absorbarces obtained. An improvement over this official method, in terms of time required, is the method of Kunze, Barkan, and Banes (1). This method eliminates the Soxhlet extraction and the Bolvent evaporation steps but maintains the 30 shakeouts, heated water bath, and large amount of sample needed. . Reserpine and rescinnamine are the principal active alkaloids in Rauwolfia serpentina, with trace amounts of other alkaloids also present (2). Any unofficial assay devised for this product would have to measure these nitrite-sensitive alkaloids in the same ratio as in the official assay. The problem, then, is essentially one of deter mining simultaneously 2 different active Ingredients present in varying proportions. Fluorometric excitation and emission spectra of both reserpine and rescinnamine derivatives have been published (3, 4), Both alkaloids have identically shaped emission spectra with their maximum emissions at the same wavelength (Fig. 1). The excitation spectra (Fig. 2) of the 2 alkaloids are not identically shaped but do have the maximum fluores cences at the same wavelength. Work in this laboratory also demonstrated that, if the excitation wavelength is held at this maximum, the' ratio t. ^ ,i 1 ] ,imwiBfii 11 mi-- DSW 033457 STLCOPCB4017419 */ 289 . FIG, l--Emission scan of rescinnamine (----) and reserpine (------- ), 420-660 nm (both compounds about 0.2 pg/ml). FIG. 2--Excitation scan of res- cinnamine (------ ) and reserpine (...-- ), 420 660 nm (both compound a about 0.2 p.g/ml). of the fluorometric responses of the nitrous acid derivatives of these 2 alkaloids are in the same ratio as their absorbances at 390 nm. This information indicated that a fluorometric method for Rauwolfia serpen tina was feasible. The nitrous acid derivative, thought to be the 3-dehydro form of the parent molecule (Fig. 3) is about 12 times as fluorescent as the parent molecule (5). The difference in spectra between the nitrous acid derivative and the parent molecule is probably due to epimerization at C3 and unsaturation in' ring C. The strong fluorescence of this derivative allows one to use a much smaller sample and eliminates the solvent evaporation step. The smaller sample can be refluxed directly in the solvent, thus eliminating the Soxhlet extraction apparatus. The derivative formation follows the USP XVII method for reserpine. These conditions have been established as optimum for the reserpine assay (6). Work in this laboratory indicates that these conditions are also suitable for the determination of rescinnamine even though it has a slightly different derivative formation rate as shown in Fig. 4. DSW 033458 STLCOPCB4017420 290 Reserpine 3-Dehydroreserpine FIG, 3--Derivative formation of reserpine. Rauwolfia serpentina tablets are frequently coated with a dye which is not removed in the sample cleanup. The presence of dyes can.lead to low results by absorption of light at the activation and/or emission wavelengths. An internal, standard is incorporated in this assay to compensate for this absorption. A sample blank is also employed to correct for fluorescing products, such as oxidation products of reserpine and rescinnamine, originally present :'.n the sample and not removed in the cleanup. Method Reagents (a) Methanolic HC1.--Add 25 ml concentrated HC1 to 75 ml methanol Cool to room temperature before use. (b) Sodium nitrite solution.--Dissolve 300 mg NaN02 in 50 ml water and dilute to 100 ml with methanol* Prepare fresh dally. (c) Sulfamic acid solution.--Dissolve 5 g sulfamic acid in 100 ml water. (d) Standard solution.--(A) Dissolve 6.25 mg reserpine in 10 ml CHClo and dilute to 100 ml with methanol. (B) Dilute 10 ml (A) to 100 ml vdth methanol. () Dilute 10 ml (B) to 100 ml with methanol. Solutions (B) and (C) are stable at least 1 month if kept in the dark. Apparatus Chromatographic column.--Lower layer: 3 g Celite plus 2 ml saturated NaHCOj solution. Upper layer: 3 g Celite plus 2 ml 0.5N[ h2so^. * DSW 033459 i ....,'jr.iiga '|iy-Tn STLCOPCB4017421 291 2 1 ! & Time, minutes FIG. 4--Derivative formation rate for reserpine (1) and rescinnamine (2). Procedure Powder a minimum of 20 tablets and pass through 60 mesh sieve. Mix composite thoroughly. Weigh amount of sample equivalent to ca 250 pg total alkaloids Into 250 ml Erlenmeyer flask equipped with air condenser. Add 100 ml 95% ethanol and reflux on steam bath 30 60 min. Cool to room temperature, add 100 ml CIICI3, stopper securely, and shake solution vigorously 30 min. Transfer to 250 ml volumetric flask, dilute to volume with CHCI3, and filter through paper. Transfer 50 ml aliquot of filtrate to 250 ml separatory funnel containing 200 ml 0.5N H2SO4 and shake funnel vigorously 2 min. Drain lower layer (may be slightly turbid) onto chromatographic column. Collect eluant in 200 ml volumetric flask containing 50 ml methanol. Extract aqueous solution in separatory funnel with 4 portions of 25 ml CHCI3, draining each extract onto column after previous one enters column. Dilute eluant to volume with CHCI3 and mix. DSW 033460 STLCOPCB4017422 292 FIG, 5--Emission spectrum of a typi cal sample of Rauwolfia serpentina, 420-660 nra. FIG^ 6--Excitation spectrum of a typical sample of Rauwolfia serpentina. 260-480 nm. ` Transfer 25 ml aliquots of this solution to each of three 50 ml volumetric flasks labeled A, 13, and C_. To flasks A and 1$ add 10 ml methanol. To flask C add 10 ml standard solution . Add 5 ml 50% aqueous methanol to flask A. To flasks 13 and add 5 ml NaNC>2 solution. Add 5 ml methanollc HC1 to all 3 flasks. Mix thoroughly. After 30 min, add 2.5 ml sulfamic acid solution to all 3 flasks and dilute'samples to volume with methanol. Mix and determine fluores cence after 15 min, mixing and venting solution to dispel nitrogen during this time. Use the following Instrumental conditions: activation wavelength 400 nm (uncorrected), emission wavelength 502 nm (uncorrected). Use minimum activation and emission slit widths consistent with good quantitation according to manufacturer (on our Hitachi Perkin-Elmer MPF-2A, this is 10 nm and 12 nm, respectively). The sensitivity used is dependent upon slit widths. X Reserpine - rescinnamine group alkaloids Sample B - Sample Blank A mg Standard (Av. g/Tablet) x 4 Standard C - Sample B X g Sample X mg Tablet declaration DSW 033461 STLCOPCB4017423 A*.a 293 Results Figures 5 and 6 show typical emission and excitation spectra of Rauwolfia serpentina samples. Results are presented in Table 1 for the analysis of tablets by both the NF XII and fluorometric methods. Table 1. Comparison of NF XII and fluorometric method Sampled. 1 2 3 4 5 6 NF XII 0.192 Rauwolfia serpentina, % Fluorometric Method 0.191 0.192 0.193 ' 0.190 0.150 0.152 0.138 0.140 0.160 0.162 0.150 0.152 0.186 0.188 ^Sample 1 is Rauwolfia serpentina NF. All other samples are red sugar-coated tablets. REFERENCES (1) Kunze, F.M., Barkan, S., and Banes, D., .J. Ass. Off. Anal. Chem. 51, 157-159 (1968). (2) Banes, D., Wolff, J., Fallscheer, H.O., and Carol, J., Pharm. Ass., Sci. Ed. 45, 708 (1956). Amer. (3) Mader, W.J., Haycock, R.P., Sheth, P.B., and Connolly, R.J., J. Ass. Off. Anal. Chem. 43, 291-295 (I960). (4) Missan, S.R., Ciaccio, L.L., McMullen, W.H., Pazdera, H.J., and Grenfell, T.C., J_. Amer. Pharm. Ass., Sci. Ed. 49, 7 (I960). (5) Haycock, R.P., Sheth, P.B., and Mader, W.J., J. Amer. Pharm. Ass., Sci. Ed. 48, 479 (1959). (6) Mader, W.J., Haycock, R.P., Sheth, P.B., and Connolly, R.J., J^. Ass. Off. Anal. Chem. 44, 13-17 (1961). ii--wwji. DSW 033462 ------ STLCOPCB4017424 Ince.rbureau By-Lines No. 6 May 1970 APPLICATION OF NEUTRON ACTIVATION ANALYSIS TO FOOD PRODUCTS: A BIBLIOGRAPHY J? ('-'n James T. Tanner and Melvin Friedman Division of Food Chemistry and Technology For about 4 years the Food and Drug Administration, utilizing the Naval Research Laboratory reactor, has applied neutron activa tion analysis to various samples of foods, drugs, and biological als. Neutron activation analysis is especially attractive for measuring both trace and major amounts of elements in foods: 0) It is a sensitive method of analysis; (2) it is free of ' reagent and laboratory contamination; and (3) .the method of measure ment depends on the nuclear properties of the element and consequently matrix effects are unimportant. In the past 10 years many research workers have come to realize the importance of the application of neutron activation analysis to food products and so the literature in the field has burgeoned. This bibliography was compiled so that research workers interested in the application of neutron activation analysis to foods could have more ready access to relevant literature. /' This bibliography derives from a search of Nuclear Science Abstracts through November 30, 1969 and therefore covers the literature through September 1969. The key words used were: activation analysis, animal feeds, dairy products, diet, food, food chains, fruits, meats, nutrients, and vegetables. 1. Adamek, A., Obrcesnik, I., Kukula, F., and Krivanek, M., Substoichiometric determination of traces of thallium and platinum by activation analysis. Nucl. Activ. Tech. Life Sci. Proc. Symp. Amsterdam 1967 pp, 189rl94. - 2. Bergner, K. G., Problems and methods in food analysis. Deut. Apoth.Ztg. 107, 215-220 (1967). 3. Buchanan, J. D,, Activation analysis with a triga reactor. Proc. Inter. Conf. Mod. Trends Activation Anal. College Station, Tex. 1961 , pp. 72-77. 4. Buchanan, J. D., and Guinn, V. P., Analysis of foods by neutronactivation techniques. Food Technol. 17, 17-22 (1963). ; DSW 033463 STLCOPCB4017425 5. Ching, H. S., Ke, C. H., and Lin, C. Y., Determination of bromine and iodine in podium glutamate by neutron activation analysis. J. ChlneBe Cheia. Soc. (Taiwan) 10, 92-100 (1963). 6. Christell, R., Erwall, L. G., LJanggren, K., Sjastrand, B., and Westcrraark, T., Methods of activation analysis for mercury in the biosphere and in foods. Proc. Intern. Conf. Modern Trends Activation Anal. College Station, Tex. 1965. pp. 380-382. 7. Das, H. A., Hoede, D., and Zonderhuis, J., Determination of bromine in wheat, flour, and bread by neutron activation analysis. Reacter Centrum Nederland, Petten, Rept. No. RCH-106 1969. 8. Das, H. A., Van Raaphorst, J. G., Hoede, D., and Zonderhuis, J., The determination of mercury in potato flour. Intern. J_. Appl. Radiation Isotopes 17, 252-253 (1966). 9. Das, H. A., Van Raaphorst, J. G., Menger, J. W., and Galesloot, T. E., Manganese determinations at the nanogram level in dairy products. Nucl. Activ. Tech. Life Sci. PJoc. Symp. Amsterdam 1967 pp. 379-387. 10. Fer, A., nd Fotjrcy, A., Rapid simultaneous determination of traces of bromine and arsenic in plant materials using neutron activation and distillation. Nucl. Appl. 360-364 (1969). 11. Fourcy, A., Use of activation analysis for agricultural products - and foodstuffs. Bull. Inform. Sci. Tech. (Paris) No. 99, 57-70 (1965) (French; English summary). 12. Geisman, J. R., Carey, W. E., Gould, W. A., and Alban, E. K., Distribution of arsenic residues by activation analysis. .J. Food Sci. 34, 295-298 (1969). 13. Grummitt, W. E., and Lahaie, G., Strontium, barium, and calcium in some components of human diet. At. Energy Can. Ltd. AECL-1680 1963. 14. Guinn, V. P., Activation analysis in the petroleum and chemical industry. Activation Analysis, Principles and Applications, Lenihan, J. M. A., and Thomson, S. J. (Eds.), Academic Press, New York, 1965, 129-132. 15. Guinn, V. P., Neutron activation analysis and its application to the analysis of food products. .J. Amer. Oil Chem. Soc. 45, 767--774 (1968). DSW 033464 STLCOPCB4017426 296 16. Haller, W. A., Raucitelll, L. A., and Cooper, J, A., Instrumental determination of trace elements in plant tissue by neutron activation analysis and Ge(Li) gamma-ray spectrometry. J.. Agr. Food Chem. 16, 1036-1040 (1968). 17. Hoffman, C. M., Brunelle, R. L., Pro, M. J., and Martin, G. E., Determination of trace component distribution in illicit spirits by neutron activation analysis (NAA), atomic absorption (AA), and gas-liquid chromotography (GLC). J^. Ass. Of f. Anal. Chem. 51, 580-586 (1968). 18. Kim, C., and Silverman, J., Mercury content of worldwide samples of wheat. Trans. Amer. Nucl. Soc. 11, 54 (1968). 19 Koch, R. C., and Roesmer, J., Application of activation analysis to the determination of trace elements in meat. Proc. Intern. . Conf. Mod. Trends Activation Anal. College Station, Tex. 1961, pp. 95^101. 20. Koch, R. C., and Roesmer, J., Application of activation analysis to the determination of trace element concentrations in meat. Nucl. Scl. Eng. Corp. Rept. No. NSEC-56 1961. % 21. Koch, R. C., and Roesmer, J., Application of activation analysis to the determination of trace element concentrations in meat. J. Food Sci. 27_y 309-320 (1962). 22. Kosta, L., and Byrne, A. R., Activation analysis for mercury in biological samples at nanogram levels. Talanta 16, 1297-1303 (1969). 23. Kosta, L., Ravnik, V., and Dumanovic, J., Determination of nitrogen in plant seeds by fast neutron activation analysis. Panel Meeting .on New Approaches to Breeding for Improved Plant Protein, Roestanga, Sweden, 1969, pp. 161-168. 24. Krivanek, M., and Kukula, F., Substoichiometric determination of platinum by activation analysis. Isotopenpraxis 3, 441-443 (1967) (Russian). 25. Kruger, P., and Gruverman, I. J., Neutron activation analysis for characterization of induced activities in irradiated foods. Proc. Intern. Conf. Mod. Trends Activation Anal. College Station, Tex. 1961, pp. 46-49* 26. Lambert, J. P. F., and Simpson, R. E., Note on the analysis of nutrient broth by neutron activation analysis. J_. Ass. Off. Anal. Chem. 51, 999-1002 (1968). . 27. Leddicotte, G. W., Ultratrace-element research in the life sciences using activation analysis. Isotopes Radiation Technol. 5^ 200-206 (1968). DSW 033465 1 STLCOPCB4017427 297 28. Lee, B. K., and Murphy, G. , Determination of arGenic content of American cigarettes by neutron activation analysis. Cancer 23, 1315-1317 (1969). 29. Magno, P. J., and Knowles, F. E., Jr., Determination of strontium in environmental media using neutron activation. Anal. Chew. 37, 1112-1115 (1965). 30. Malvano, R., and Grosso, P., Iodine activation analysis in materials of biological Interest. J_. Nucl. Biol. Med. 12, 86 (1968). 31. McConnell, K. P., Use of activation analysis in studies of selenium in the mammalian organism. Proc. Intern. Conf. Mod. Trends Activation Anal. College Station, Tex. 1961, pp. 137-140. 32. Meinke, W. W., Does irradiation induce radioactivity in food. Nucleonics 12(10), 37-39 (1954). 33. Mercer, W. A., Application of radiochemical techniques in food processing research. Radioisotope tracer techniques in evaluation and improvement of industry practices for removal of pesticide residues from foods. Natl. Canners Ass. West. Res. Lab. Berkeley, Calif. Rept. No. SAN-1022 1963. 34. Moeller, D. W., and Leddlcotte, G. W., Neutron activation analysis of whole milk for stable strontium. Oak Ridge Natl. Lab. Rept. 0RNL-2866 1960, pp. 22, 29. 35. Mollnski, V. J., Wahl, W. H., and Strain, W. H., Analysis of vanadium in milk powder by neutron-activation analysis using a rapid radiochemical separation of 3.77~minute vanadium-52. Trans. Anier. 'Nucl. Soc. 6y 398 (1963). 36. Nishlgaki, S., Activation analysis in soil/plant relation studies in South-East Asia. Plant Nutrient Supply and Movement, IAEA Vienna, Technical Report Series No. 48, 122-124 (1965). 37. Prapuolenls, A. A., and Bakas, J. M., The determination of phosphorus and nitrogen in herbage flour by fast neutron activation analysis. Radiochem. Radioanal. Letters 1, 19-23 (1969). 38. Rarbe, R., Determination of total strontium in vegetables, comparison of activation analysis with flame photometry. Grenoble Untv. France Rept. No. NP-17124 1966 (French). 39. Rayudu, G. V. S., Tiefenbnch, B., and Jervis, R. E., Neutron activation determination of trace mercury in Canadian foods. Trans. Amer. Nucl. Soc. 11, 54-55 (1968). DSW 033466 STLCOPCB4017428 298 40. Rossi, M. L., D' Agastino, M. D., Mostrand, J. W., Jr., and Favale, A. J., Activation research in the aerospace industry. Proc. Intern. Conf. Mod. Trends Activation Anal. College .Station, Tex. 1961, pp. 114-118. 41. Samuelsson, E.,G. Determination of trace elements in milk and milk products by means of neutron activation analysis. Radioisotopes and Radiation in Dairy Science and Technology, IAEA, Vienna, 1966, pp. 221-237. 42. Shinbori, Y., Radioactivation analysis of trace elements in refined soybean oils. I. Iron, cobalt, and nickel Yakugaku 17, 430-435 (1965) (Japanese). 43. Shinbori, Y.,and Kuwahara, H., Radioactivation analysis of trace arsenic in refined soybean oils, sunflower oils, and rape, seed oils. Yakugaku 18, 147-148 (1969) (Japanese). 44. Shinbori, Y., and Tashio, Y., Radioactivation analysis of trace elements in refined soybean oils. 2. Determination of copper and zinc. Yakugaku 17, 606-610 (1968) (Japanese). 45. Smales, A. A., and Pate, B. D., The determination of sub-microgram quantities 6f arsenic by radioactivation. III. The determination of arsenic in biological material. Analyst 77, 196-202 (1952). 46. Souliotis, A. G., Combined radiochemical - neutron activation . analysis method for the determination of sulfur and phosphorus in high-purity paper and beer. Anal. Chem. 36, 811-814 (1964). 47. - Souliotis, A. G., Grimanis, A. P., and Tsanon, N. A., Determination of chloride in beer by radioactivation analysis. Analyst 90, 499-501 (1965). 48J S^ronk, N., Nuclear activation in the animal sciences. Nucl. Activ. Tech. Life Sci. Proc. Symp. Amsterdam 1967, pp. 335-352. 49. Union Carbide, Radioisotope sales campaigns opened by G.E. and U.C. U.C. expects to quadruple its analysis business. Nucleonics 21(2), 28 (1963). 50. Wood, D. E., Fast neutron activation analysis for nitrogen in grain products. Kaman Nucl. Colorado Springs, Colo. Rept. No. KN-65-186, 1965. 51. Wood, D. E., Liquid-loop activation analysis system. Trans. Amer. Nucl. Soc. 10, 451 (1967). * 52. Yule, H. P., Reactor neutron activation analysis instrumental sensitivities in six matrix materials. Anal. Chem. 38, 818-821 (1966). KWa.'"* ~ i* T.TJ.T'fgfr DSW 033467 "* STLCOPCB4017429 299 Interbur- \tj By-Linc.s No. 5 March 3973 P OLAROGR AT]11C DETERUINATION OF NITRATES IN AQUEOUS MEDIA CONTAINING NITRITES Al.beru 7... Woodson, Chicago District A dr.'o; formulated to contain the following ingredients per tab.lo:: . ... assayed for nitrate and nitrite content: Sodiu.-i nitrite ............................................................ IV!. - :n- ium nitrate-. ..................................................... Po..:!. Ext,Echinaces ................................................ Pov;J. Ext.Chionaiitlvus ........................................... Po. d, Ext.Iris ...................... Sodivua Glycocholate ............................. 65 mg 135 mg 6.5 mg 6.5 mg 6.5 mg 6.5 rag. The nitrite was satisfactorily assayed by an AOAC colorimetric procedure (1). For the assay of the nitrate concentration the phenoldieulfonic acid procedure (2) was modified to eliminate the interference of nitrite ions. This modification consisted of treating the acidified solution of the sample with urea, which destroys the nitrite ion by convert;-'.g it to nitrogen. The nitrate assay value obtained by this modified procedure was low: 75% of the label declaration. For a check analysis, the author successfully utilized aqueous polarography for the nitrate assay. This polarographic assay is based on the catalytic effect of the nitrate concentration on the polarographic reduction wave of uranium (3). A 2 x 10 -4M solution of uranyl acetate, UOs(C2H3Os)e, in O.OlM KC1-0.1M KGl yields two polarographic reduction waves at approximate half wave potentials -0,2 and -0.9 v vs. the standard calomel electrode. The wave at.-0.2 v represents the reduction of uranium (+6) to uranium (+5); the wave at -0.9 v represents the reduction of uranium (+5) to uranium (+3) (3). In the presence of nitrate ions the uranium wave at -0.9 increases (3); as the uranium ions are reduced, these reduced ions are immediately reoxidized by the nitrate ions. These reoxidized uranium ions are reduced again and this pattern of polarographic reductionnitrate oxidation-polarographic reduction is continued until the aolution has been depleted of the oxidizer, the nitrate ions. The net result is an increase in the height of the second wave in the polarographic reduction, proflie o uranium. This catalytic effect of the nitrate ion is proportional to the concentration of nitrate ions as low as 5 x 10" (3). DSW 033468 STLCOPCB4017430 300 The nitrite ion in aqueous acid media forms nitrous acid, which is polarographically reducible at -1.0 v. Therefore, any polarographic assay of a mixture of nitrate and nitrite ions would be inaccurate because of the close proximity of the tiro half-wave potentials: -0,9 v for the nitrate ion and -1,0 v for the nitrite ion. However, since nitrous acid is easily destroyed by sulfamic acid (it converts nitrous acid to nitrogen), the addition of sulfamic acid to the solution before polarography eliminates the interference of the nitrite ion (3). Method Reagents and Apparatus (a) Sulfamic acid solution.--About 0.75M. (b) Uranyl acetate.--UO^CCoH^Oo)o.2Ho0. Fisher Certified Reagent. (c) Potassium nitrate.--Fisher Primary Standard. (d) Sargent XV polarograph.--With standard calomel reference electrode. Solutions (a) Polarographlc electrolyte.--Dissolve 86.9 mg uranyl acetate in 1 L solution containing O.OlM HCl and 0.1M KC1, The uranyl acetate concentration of this solution is 2 x 10"^M. . (b) Standard potassium nitrate.--Dissolve 97.8 mg primary standard In 100 ml water. This solution contains 0.978 mg KN03/ml. Procedure Accurately weigh portion of powdered sample equivalent to ca 130 mg potassium nitrate into 100 ml volumetric flask. Add ca 30 ml water and shake on mechanical shaker 15 min. Dilute with water to volume, mix well, and filter. Add 2 ml aliquot of filtered sample solution, 1 ml water, 2 ml sulfamic acid solution, and 15 ml polarographlc electrolyte to small Grlenmeyer flask. Mix well, let stand 10 min, de-aerate with nitrogen 5 min, and then polarograph. Scrub nitrogen before introduction into polarographlc cell by passing it through scrubber containing polarographlc electrolyte. Determine recovery as follows: Mix 2 ml filtered sample solution, 1 ml standard potassium nitrape solution, 2 ml sulfamic acid solution, and 15 ml polarographlc electrolyte. Run sample and recovery determinations in triplicate. Plot height of diffusion current vs. mg potassium nitrate/ml. Measure diffusion current at -1.1 v as indicated in Fig. 1. --------- ------ ----------....................... " --.......... ........ ............ DSW 033469 STLCOPCB4017431 301 FIG. l--Second wave in the polarographic reduction profile . of uranium. Results and Discussion The results of the sample assays are shown in Table 1; the results of the recovery determinations are shown in Table 2. These data indicate that this procedure may be successfully employed for the polarographic determination of nitrates in the presence of nitrites. The preparation of a standard potassium nitrate curve shows the linearity of the nitrate concentration-wave height profile in the range of 0.078-0.195 mg/ml (Fig. 2). DSW 033470 iKBjB'i Si j.jynwwiaLir*iMammmmnt'Jxi~iiujjuismk!-i -j-.ji.-mww. r- STLCOPCB4017432 302 Table 1. Results of polarographic assay of sample S ample E 1/2, volt ^/Tablet Found Declared % of Declaration 1 -0.90 129.1 130 2 -0.90 132.0 130 3 -0.90 130.3 130 Av * -0.90 130.5 130 99.3 101.5 100.2 100.3 A typical polarographic wave obtained with the sample solution is shown in Fig, 1. The wave at -0.2 v, which represents the reduction of uranium (46) to uranium (4-5), is not seen on this typical polarogram because the sensitivity of the Sargent XV has been lowered in order to confine the wave at -0.9 v to the available chart space. If the sensitivity of the instrument were set at .0,04 jrA/mm, the wave at -0.2 v would appear, but the wave at -0.9 v would be off the chart. Vave H t, -p,------ -- STLCOPCB4017433 Table 2. Assay Results of recovery of nitrate by polaror.raphic assay E 1/2, volt ____ E2. KNO-, Added Found % Recovery 1 -0.91 0.978 0.96 98.2 2 -0.92 0.978 0.98 100.2 3 -0.91 0.978 0.96 98.2 Av. -0.913 0.978 0.967 98,9 References (1) Official Methods of Analysis. 10th Ed., AOAC, Washington, D.C., 1965, secs. 23.013-23.014. (2) Official Methods of Analysis, 10th Ed., secs. 32,306-32,308. (3) Brezina, M. and Zuman, P., Polaroaraphy In Medicine, Biochemistry and Pharmacy, Interscience Publishers, Inc., New York, 1958, pp. Ill, 112, 114, 115. DSW 033472 rv-ivnjB STLCOPCB4017434 Tho.se shrimp (white, brown, and pink) were commercially available raw, frozen, peeled, and deveinod. They were hard frozen when received. Shrimp were thawed and individually classified organoleptically. Individual 50 g portions of Class I, II, or HI were weighed and used to determine pH, volatile base, and indole. When determina tions could not be made on the same day as the organoleptic examination, individual 50 g portions were immediately hard frozen and stored; when time permitted, they were thawed, classified organoleptically, and used to determine pH, volatile base, and indole. In no case did more than a week elapse between the original organoleptic examination and other tests. Since published procedures were not available for determining a series of indices on the same 50 g portion,established methods for indole (2) and volatile bases (3)*were combined and modified as follows: (A) Distillation procedure: (1) A calcium hydroxide trap was placed between distillation flask and condenser. (2) Antifoam A spray was used instead of alcohol in the distillation flask. (B) Volatile bases (3): The distillate was collected in 0.1N HC1 and back-titrated with 0.1N NaOH to pH 7, using a pH meter with a glees and calomel electrode. (C) Indole (4): (1) The titrated volatile bases distillate was quantitatively transferred to a 1000 ml separatory funnel containing 10. ml of 10% 11C1 and 10 ml of a saturated solution of sodium sulfate. Three 1-minute extractions were made with 30 ml portions of CHCI3. The CHCI3 extracts were drained into a 125 ml separatory funnel through an absorbent cotton plug. (2) Color was developed as in the established indole method. Reagents and Apparatus Experimental (a) Color reagent, purified acetic acid, dilute hydrochloric acid, and indole standard solution.--All from sec. 18.036 (4). (b) Distillation apparatus.--(1) A separate steam generator should be used for each unit. Steam generator may be made from 2 L Erlenmeyer flask connected to all-glass steam distillation apparatus, ammonia distilling apparatus (JD-1710 Scientific Glass Apparatus Co., Inc., Bloomfield, N. J., or equivalent with minimum use of rubber tubing). (2) Distilling flask. (3) Trap flask, 800 ml Kjeldahl, connected through a (4) spray trap via rubber tubing to a trap flask which is connected to a (5) straight bore condenser through the spray trap. An 800 ml beaker is an effective receiver (Fig. 1). The 5 Joint is cut away from the spray trap on the sample flask and a rubber tube is used to connect the sample spray trap to the spray trap on the trap flask. DSW 033474 STLCOPCB4017436 300 PIG, 1--Schematic of distillation apparatus. . (c) pH meter.--Reading to two decimal places (glass and calomel electrode). (d) Calcium hydroxide.--(Baker analyzed reagent 1372 or equiva lent). 15 g of Ca(OH)2is dissolved in 1000 ml of water. 150 ml is used in the trap flask for each determination. *_ Organoleptic Examination The shrimp were thawed, the organoleptic examination was performed to note classification, and samples were weighed in individual 50 g portions. pH Determination The 50 g portions of shrimp were placed in a 1 qt. Waring Blendor and blended for 2-3 min. The pH. of the blended shrimp was taken with a pH meter (glass and calomel electrode) and recorded to two decimal places. Determination of Volatile Bases Eighty to 100 ml of water and a 10 second burst of Dow Corning Antifoam A pressurized spray was added to the previously blended 50 g portion of shrimp and blended for 2 min. The blend was quanti tatively transferred to a distillation apparatus (Fig. 1). A 500 ml portion was distilled into a beaker containing 50 ml of 0.1N HC1 fcondenser tip is immersed into the O.lhJ HC1 in the receiving beaker). (Note: The calcium hydroxide solution in the trap flask DSW 033475 i STLCOPCB4017437 307 # .J ) must be boiling before distillation begins.) The distillate was titrated to pH 7 with 0.1N NaOU (pH meter), corrected for back titration, and the value multiplied by 20 to correct to the quantity of 0.01N NaOH in 100 g of shrimp ("volatile bases"). Indole Determination The titrated distillate from the volatile base determination was transferred to a 1000 ml separatory funnel containing 10 ml of a saturated solution of sodium sulfate and 10 ml of 10% HC1. The aqueous phase was extracted 1 rain with three 30 ml portions of CHCI3 (USP). The CHClo was drained through an absorbent cotton plug in the stem of the 1000 ml separatory funnel into a 125 ml separatory funnel containing 10 ml of the color reagent and shaken for 2 min. Then 9 ml of color reagent (bottom layer) was drained into a 50 ml glass-stoppered cylinder and diluted to 50 ml with acetic acid. The color developed immediately upon shaking. Using a visible recording spectrophotometer, the spectrum was recorded from 650 to 425 am against a reagent blank. The quantitative absorbance maximum was read at 567 nm and a background correction was made . by drawing a straight line from the absorbance peak at 650 nm to that t 425 nm. Background absorbance (the point a<: which the line crosses 567 nm) is subtracted from total absorbance at 567 nm. Indole standard solutions containing 0, 20, 30, and 40 gg indole were prepared and taken through the procedure, and an indole standard curve was prepared. The amount -of indole in the shrimp sample was calculated from the standard Indole curve and multiplied by a factor of 2 to obtain gg indole in 100 g of shrimp Recovery of indole by this method is 96.9 --100% if the calcium hydroxide trap is boiling vigorously before distillation is begun. If the calcium hydroxide in the trap is not boiling vigorously, Indole recovery values drop to 85 ~ 90%. Results and Discussion The results of the determination of the three classes of organoleptic shrimp are listed in Table 1. pH, volatile bases, and indole were determined <w 35 portions of white, brown, or pink shrimp in Class 1, 15 portions in Class II, and 23 portions in Class III. The pH, Indole content, and volatile bases values show a steady increase as the shrimp progress from Class I through Class III. Table 1 also shows that the indices overlap into several organoleptic classes. Some indices do not properly represent the organoleptic classification. The reasons for this deviation are not known. _ . DSW 033476 wn'1.! '* iiuipMM;irM&`|'r-- -------- ...... .. _ . STLCOPCB4017438 308 Table 1. Experimental data on white, brown, and pink shrimp (not listed separately) Indole, Volatile Bases * pH pg/100 g ml 0.01.H NaOH/LOO g Organoleptic Class I 7.13 8.4 7.08 9.6 7.12 0 7.80 10 7.87 20 7.07 8 7.12 8.4 7.09 0 7.10 8.4 7.09 8.8 7.08 8.0 7.13 0 7.40 12.4 7.20 8.0 7.25 8.0 7.30 0 7.48 14.0 7.30 3.0 . 7.52 0 7.43 0 7.35 0 7.48 0 7.30 0 7.46 0 7.70 8 7.57 '4 7.26 0 8.03 11 7.31 0 . . 7.37 0 7.47 0 7.53 0 7.62 11.4 7.43 14.0 7.40 10.4 173 163 17 143 208 260 264 216 163 167 192 174 175 125 142 211 205 192 33 61 68 52 37 52 150 87 119 310 297 101 166 162 203 72 65 Tndole, Volatile Bases, pH pg/100 g ml 0.01N NaOH/100 g Organoleptic Class II 7.59 7.56 7.57 7.42 7.82 7.50 7.72 7.81 7.72 7.86 7.81 7.45 7.52 7.58 7.46 46.2 71.2 40.0 44.0 6.0 64 24 15 30.4 24 35 28.4 17 30.6 29.2 268 276 255 274 363 258 87 212 270 . 326 234 222 239 224 209 Organolepti c Class III 7.67 7.91 7.99 7.81 7.98 7.25 7.90 7.87 7.45 7.98 8.22 8.00 8.02 7.95 7.70 7.72 7.69 7.41 7.70 7.72 7.60 7.83 7.76* 90.0 156.0 70.0 400.0 14.0 54.0 62.0 25.0 46.0 19.0 155.8 171.2 42.0 26.0 128.6 120.4 102.4 28.0 90 54.4 74.0 115.0 94.0 368 366 251 422 165 298 277 144 277 206 149 326 252 230 359 399 340 468 503 423 660 662 715 DSW 033477 STLCOPCB4017439 309 Table 2. Organoleptic and chemical indices of decomposition In shrimp (from Table 1) Class I Class II Class III r.H iv. liA'l'?, g/100 g Aw. .. Usage 7.37 7.07 - 8.03 5.5 0-20 Volatile liases, ml 0.01N NaOH Av. . lor.je.. 155 33 - 310 7.63 7.42 - 7.86 33.6 6.0 - 71.2 7.79 7.25 - 8.22 110.4 14.0 - 400 248 87 - 363 359 144 - 715 Table 2 summarizes the results for pH, indole content, and volatile bases obtained oil the 3 organoleptic classes of the shrimp. Separate lota of brown shrimp and pink shrimp were examined by the organoleptic technique previously discussed. The separated shrimp samples were examined immediately and then again after the same lot of shrimp was allowed to decompose in plastic bag9 at room temperature for 24 hr. The values for organoleptic class, pH, indole content, and volatile bases on the separated brown and pink shrimp increased as shown in Tables 3 and 4. Since this study was conducted on commercially prepared shrimp, all previous history of the shrimp is unknown. The deviations of some values could be the result of chemicals used on the shrimp, variations with type of shrimp, and general handling before and after freezing. Conclusion Each set of values reveals a noticeable upward trend as the shrimp decompose. These results are of value as additional data to help correlate the findings from organoleptic determination of shrimp quality. The 4 indices should be further evaluated on individual species of commercial shrimp under known conditions and beginning with live shrimp. DSW 033478 -*rrr STLCOPCB4017440 Table 3. Organoleptic class, pH, indole content, and volatile base values for brown shrimp and the same lot held 24 hr at room temperature Organoleptic pH Class Indole, ug/100 g Fresh Shrimp Volatile Bases, ml 0.01N NaOH/100 g 7.40 7.20 7.25 7.30 7.48 7.30 Av. 7.32 1 I I I I I 12*4 8.0 8.0 0.0 14.0 3.0 7.56 Stored Shrimp , 175 125 142 211 . . 205 192 175 7.41 7.70 7.72 7 <76 7.83 7.76 Av. 7.70 III HI III III in iii 28.0 90.0 54.4 74.0 115.0 94.0 75.9 468 503 423 660 662 715 572 DSW 033479 ~rrr. I STLCOPCB4017441 311 Table 4. Organoleptic class, pH, indole content, and volatile base values for pink shrimp and the came lot held 24 hr at room temperature Organoleptic pH Class Indole, ug/100 g Fresh Shrimp Volatile Bases, ml 0.0IN NaOH/100 g 7.52 7.43 7.35 7.48 7.30 7.46 Av. 7.42 I I I I I I '' 7.57 7.54 7.60 7.56 7.62 7.70 Av. 7.60 . Ill III III III III III 0 0 0 0 0 0 0 Stored Shrimp 12 16 14 26 20 26 19 33 61 68 52 37 . 52 50 131 159 139 180 208 155 162 i QSW 033460 STLCOPCB4017442 References (1) Campbell, C., J. Ass. Off. Anal. Chem. 45, 731-732 (1962). (2) Duggan, R. E., and Strasburger, L. W., J. Ass. Off. Anal. Chem. 29, 177-188 (1945). (3) Hi.llig, F., Shelton, L. R. , Jr., Loughrey, J. H., and Eisner, J., J. Ass. Off. Anal. Chem. 41, 763-776 (1958). (4) Official Methods of Analysis, 10th Ed., Association of Official Agricultural Chemists, Washington, D. C., 1965, secs. 18.036-18.038. * m+r V.'TT- CSW 033481 fM * i*l w m iiii-TI STLCOPCB4017443 313 Interbureau By-Lines No. 6 May 1970 DIFFERENTIAL EFFECTS OF DDT AND POLYCHLORINATED BIPHENYLS ON THE CENTRAL NERVOUS SYSTEM Thomas J. Sobotka, Division of Pesticide Chemistry and Toxicology Refined chemical procedures have only recently been developed which enable DDT to be differentiated from polychlorinated biphenyls (PCB) in single samples (personal communication from Judith Armour, DPCT, to be published in JAOAC, July 1970). Because these two classes of compounds are difficult to separate and because they are both found in wildlife species, it is possible that effects previously attributed to DDT may in fact be due to Aroclor residues. The present work was undertaken to determine whether central behavioral and physiological.systems are similarly or differentially affected by DDT and polychlorinated biphenyls. Two representative samples of the PCB class were investigated, namely, Aroclor 1260 and Aroclor 1254. Methods Adult male*mice (Flander's Research Farm) were used throughout the study. Animals were housed in groups of 15-20 with constant lighting and temperature. Food and water were provided ad libitum. All compounds were dissolved in corn oil and administered orally at volumes equivalent to 0.01 ml/g body weight. ^ Open-Field Activity (Exploratory Activity). - The apparatus to measure exploration of the DDT and Aroclor 1260 groups was different from that used to gauge exploratory activity of the Aroclor 1254 groups. Therefore, only the DDT and Aroclor 1260 groups can be validly compared. However, the data from the Aroclor 1254 groups will be presented for completeness. Exploratory behavior for the DDT and Aroclor 1260 groups was measured by the use of a large rectangular box (10 x 18 x 6") with marked grid floor. Twenty-four hours after dosing, each animal was tested individually. The number of squares traversed per minute was recorded for a 5 min period. The average minute activity was used as the exploratory activity. Exploration by the Aroclor 1254 groups was determined in circular photoactivity chambers (18" diameter x 15" high). Twenty-four hours after dosing, each mouse was placed in a photoactivity chamber and the number of light beams crossed per minute for 5 min was recorded. The average minute activity was used as the exploratory activity. 'WV.--. * .">* 'VO DSW 033482 . ............. - ..-w--in STLCOPCB4017444 314 In order to gauge the rate at whicn the mice were habituating to the novel environment during their 5 min exposure, the difference between the average activity of the first 2 min and the last 2 min wps calculated. A large difference (the average activity of the last 2 rain being smaller) was taken to imply a rapid suppression of motor exploration, i.e., a high degree of habituation; conversely, a smaller difference would indicate relatively little motor suppression or habituation to the novel environment. The use of a decline in exploratory activity over a period of time as an index of habituation .Is based on the methods of Carlton (1). DDT was given in doses of 0, 1.0, 10.0, and 25.0 mg/kg (total number of mice >* 60). Aroclor 1260 was administered at 0, 1.0, and 10.0 mg/kg (total number of mice = 39). Aroclor 1254 was given at doses of 0, 0.5, 1.0, and 10.0 mg/kg (total number of mice 48). Passive Avoidance. - Fear-induced suppression of motor activity (passive avoidance) was measured in a standard passive avoidance situation (2). The apparatus consisted of a small Plexiglas chamber (3.5 x 6.5" with a grid floor) adjoining a larger chamber (13.5 x 13.5" with a grid floor) with a door between them. Four hours after dosing, each mouse was placed in the small chamber facing away from the door. The door was immediately opened, thereby activating a timer. The time (latency) to enter the larger chamber was recorded. As soon as the animal stepped into this chamber, the door was closed end an 8 ma/0.2 sec shock was delivered through the grid floor. The mouse was then returned to its home cage. On the following day the animal was given a single post-ahock (fear) test. The latency to enter the large "shock" chamber was recorded but no shock was given. DDT (80 mice), Aroclor 1260 (81 mice), and Aroclor 1254 (48 mice) were administered in oil in single oral doses of 0, 0.5, 1.0, and 10.0 mg/kg. Maximum Electroshock Seizure. - Four hours after dosing, maximum electroshock seizure was Induced by a 30 ma/0.2 sec pulse delivered via saline wetted corneal electrodes. The durations of the following seizure components were measured: tonic flexion, tonic extensleny, and clonus. In addition, the ratio of tonic flexion/tonic extension was calculated. The following doses of DDT (61 mica), Aroclor 1260 (46 mice), and Aroclor 1254 (40 mice) were given: 0, 0.5, 1.0, and 10.0 mg/kg. DSW 033483 STLCOPCB4017445 FIG. 1--Effect of DDT, Aroclor 1260, and Aroclor 1254 on (A) exploratory behavior and (B) habituation (4 hr pretreatment). DSW 033484 316 Results All results are expressed as per cent of control. Figure 1A depicts the changes in exploratory activity induced by DDT and Aroclor 1260. At 1.0 and 10.0 mg/kg there does not appear to be any marked differences between the effects of the 2 compounds. The Aroclor 1260 groups do, however, tend to exhibit a slightly lower exploratory activity. A similar low exploration is seen with the Aroclor 1254 group at 1.0 mg/kg. The habituation scores seen in Fig. IB similarly do not differen tiate between DDT and Aroclor 1260. Aroclor 1254 does induce a facilitation of habituation. But this effect cannot be validly compared with the DDT or Aroclor 1260 groups since different apparatus was used. In contrast to exploratory and habituation scores, a clear distinction between DDT and both of the Aroclor compounds is seen in the passive avoidance behavior. As shown in Fig. 2, the DDT-treated mice entered the shock (stress) chamber faster, while the Aroclor 0.5 1.0 10.0 300 200 100 Per cent o f respective co n tro l Doses, mg/kg FIG. 2--Effecto of DDT, Aroclor 1260, and Aroclor 1254 on latency to enter a shock-stress chamber (all agents were given 24 hr before shock and 48 hr before testing latency to enter ' shock chamber). . DSW 033485 ' -tKtm,'WHfWU STLCOPCB4017447 Per cent o f respective co n tro l 317 FIG. 3--Effect of DDT, Aroclor 1260, and Aroclor 1254 on maximum electroshock seizure 4 hr after dosing. DSW 033486 318 1260~ and 1254-treated animals generally took a much longer time to enter the stress chamber when compared to their respective controls. Further distinction between DDT and Aroclor compounds can be seen in their effects on MES pattern (Fig. 3). Mice treated with either Aroclor 1260 or 1254 exhibited a prolonged duration of clonus (ArocJor 1260 was more effective in this than was Aroclor 1254) and an increased tonic flexion/tonic extension ratio, and tended to have a decreased tonic extensor duration. Each of these effects is the opposite of that found after DDT treatment. Animals treated with DDT had a prolonged tonic extensor phase and a depressed tonic flexion/ tonic extension ratio, and tended to have a decreased or unchanged clonic phase compared to controls. Discussion The present work has shown that DDT and polychlorinated biphenyls (specifically, Aroclor 1260 and Aroclor 1254) exert differential effects on the central nervous system. . The behavioral inhibition induced by shock stress (3) is attenuated by DDT as seen by the facilitation of entrance into the Bhock (stress) chamber. The Aroclor compounds resulted in the opposite effect. These agents prolonged the latency to enter the shock chamber, thereby enhancing the inhibitory effects of stress. The general*level of central neuronal excitability is also differentially affected. The depression of the tonic flexion/ tonic extension ratio (resulting from a decreased duration of tonic flexion and a prolongation of tonic extension) by DDT reflects an overall increase in brain excitability (4). DDT also fceteded to exert a depressant effect on the clonic phase of MES. In contrast, the Aroclor compounds increased the tonic flexion/tonic extensor ratio (resulting primarily from the decreased duration to tonic extension). This reflects an overall decrease in central physiological excitability. The clonic phase, which is thought to be due to an active inhibitory system (5), is generally prolonged by the Aroclor compounds, especially Aroclor 1260. . The possibility exists that DDT may attenuate central inhibitory systems, while polychlorinated biphenyls may enhance central inhibitory systems, but further experimentation is necessary. In summary, the present work not only has shown that the differential effects exerted by DDT and polychlorinated biphenyls distinguish these two classes of compounds, but also indicates that they exert opposite effects on the central nervous system. DSW 033487 STLCOPCB4017449 319 f ) References (1) Carlton, P., in Progress in Brain Research, Vol. 28, Bradley, P., and Fink, M. (Eds.), Elsevier, New York, 1968, pp. 48-60. (2) Weiss, J., McEwen, B., Silva, M., and Kalput, M., Science 163, 197-199 (1969). (3) Stein, L., Chemistry of Reward and Punishment: Psychopharmacology A Review of Progress 1957-1967*, Public Health Service Publication No. 1836, Efron, D. (Ed.), U. S. Government Printing Office, Washington, D. C., 1968, pp. 105-123. (4) Woodbury, D., and Vemadakis, A., in Methods in Hormone Research 5^, Dorfman, R. (Ed.), Academic Press, New York, 1966, pp, 1-57, (5) Gastaut, H., and Fischer-Williams, M., "The Physiopathology of Epileptic Seizures" in Handbook of Physiology (Neurophysiology). Section 7, Vol. 1, Field, J. (Ed.), American Physiological Society, Washington, D. C., 1959, pp. 329-363. U DSW 033488 STLCOPCB4017450 Interbureau By-Lines No. 6 May 1970 MICROBIOLOGICAL CONTAMINATION BIBLIOGRAPHY (Continued)1 Compiled by Harriet M. Oxley, Science Information Facility 1. Anonymous, Use of Disinfectants in the food industry. Voeding lechnick 3, 905-908 (1969). 2. ,V:!air, J., et al., Methods of sampling dairy products for bacteriological analysis. Ann. Nutr. 23, A5-A25 (1969). 3. Avakian, 0. A., Detection of Cl. botulinum in taw materials, partly manufactured goods and finished products of canned goods by the luminescent-serologic method. Gig. Sanit. 33, 110 (1968). 4. Basille, D., e_t al., Methods for bacteriological testing of fresh cheeses and yogurts. Ann. Nutr. 2J) (3) , A39-AL8 (1969). 5. Beers, W. H., et ajl., Isolation and characterisation of Cloetridum botulinum Type B toxin. J_. Biol. Chem. 244, 4473-4479 (1969). 6. Beliakov, V. D., et al., On food posioning caused by Salmonella amaRer. Gig. Sanit. 34, 46-48 (1969). 7. Bibergan, E. I., et al., Use of Ivanov medium in the isolation of Salmonella and Shigellae. Lab. Delo. 6_, 369 (1968). 8. Bilbrough, J., Food sterilization by microwave radiation. Non-Ioniz. Radiat. 1, 70-72 (1969). 9. Bory, J., Gases released by Clostridium oedematlens grown in a sodium thioglycolate medium under vacuum. Ann. Inst. Pasteur 11. 222-225 (1969). 10. Braun, D. D., Some ways of improving sanitary hygienic indices of articles made of low pressure polyethylene and polypropylene for use in the food industry and in private life. .J. Hyg. Epidem. 13, 254-263 (1969). . 11. Broeke, R.. Ten.Staphylococcus aureus and staphyloccal enterotoxins in dried milk. Neth. Milk Dairy J. 23, 223-224 (1969). 12. Brooks, J. B., et al., Differentiation between Clostridium sordelli and Clostridium biferraentana by gas chromatography. J_. Bact. 100, 528-530 (1969). ^"See Interbureau By-Lines 5. 229-232 (1970). DSW 033489 STLCOPCB4017451 321 i 13. Burganov, P, {'. , The evolution of botulism. V. The evolution of the pathogenic properties of Clostridium botulinum. Zh. Microbiol. 45 3-7 (1568). ' " 14. Cherubin, C. E., et al. , The cpidemioloe;v of salmonellosis in New York City. Amor. J. Epidrn. p_0, 112-125 (1969). 15. Clem, J. P., Sanitation guidelines for the breaded-shrimp industry. U. S. Pish Wildlif e Eur. Co;,..v.cr. Fish. C.irc. 308, 1-14 (1968) . 16. Davis, J. G., Microbiological standards for foods. Dab. Pract. _18, 39-44, Passim (1969). 17. Durhan, E., jet al^., Resistance of spores of Clostridium botulinum 33A to combinations of ultraviolet and gamma rays. Appl. Microbiol. 18, 44-50 (1969). 18. Forget, A., et al., Correlation between virulence and other charac teristics of Clostridium perfringens Type A. Appl. Microbiol. 18, 668-676 (1969). * 19. Foster, E. M., The problem of Salmonellae in foods. Food Technol. 23, 1178, 1180-1182 (1969). 20. Galeslott, T. E., et al., The microbiology of spray-dried milk products with special reference to Staphylococcus aureus, and Salmonella. Ned. Melk-Zuiveltijdschr. 22(4), 158-172 (1968). 21. Gimeno, E. J., et al., Study of the control of Salmonellae in meats exported from the Republic of Argentina. Bull. Office Int. Epizoot. 68, 299-306 (1967). 22. Grinmaer, T. V., Comparison of media with antibacterial preparations in the bacteriological diagnosis of dysentery. Lab. Delo. 6, 370-371 (1968). 23. Hall, J. R., Enhanced recovery of Salmonella montevideo from onion powder by the addition of potassium sulfite to lactose broth. J_. Ass. Off. Anal. Chem. 52, 940-942 (1969). 24. Harrison, J. M., ejt al., Microbiological evaluation of Pacific shrimp processing. Appl. "Microbiol. 18, 188-192 (1969). 25. fleidelbaugh, N. D., t l., Effect of processing on recovery of polio virus from inoculated foods. .J. Food Sci. 34, 239-241 (1969). 26. Holbrook, R., et al., The performance of a stable version of BairdParker medium for isolating Staphylococcus aureus. J. Appl. Bact. 32, 187-192 (1969). DSW 033490 STLCOPCB4017452 322 27. Iveson, J. B., e_t l., Strontium chloride and strontium selenite enrichment broth media in the isolation of Salmonella. J. Uyg. 67, 457-464 (1969). ' 28. Johnson, M. G., e al., Death of Salmonella typhimurium and Escherichia coll in the presence of freshly reconstituted dehydrated garlic and onion. Appl. Microbiol. 1_7, 903-905 (1969). 29. Kielwein, G., Nutrient medium for the selective cultivation of pseudomonas and aeromonads. Arch. Lebensmitte.lhyg. 2()(6), 131-133 (1969). 30. Kudo, H., Basic study of fluorescent antibody technics. Jap. J_. Clin. Path. 17, 522-529 (1969). 31. Labeyrie, S., et al., Chromogenesis of e^throgenic colonies of Pseudomonas aeruginosa in a synthetic medium. C. R. Acad. Sci. (D) 266", 1898-1900 (1968). 32. Lang, K., Culturing of salmonellae and shigellae from milk and dairy products by an enrichment technique. I. Inhibitory effect of the enrichment substrate on milk bacteria. Arch, Lebensmittclhyg. 20(6), 121-128 (1969). , ` 33. Lebert, F., ejt a_l. , Bacteriological analysis cf melted cheeses. Ann. Nutr. 23(3), A49-A80 (1969). . " 34. Mehringer, W., Packaging problems in the preservation of food by irradiation. Fette-Seifen Anstrichmettel 71, 516-521 (1969). 35. Meisel-Mikolajczyk, F., t l., Serological properties of bacterial fractions of the Clostridium perfringens type A strains causing acute food poisoning. Bull. Acad. Pol. Sci. (Biol.) 17, 227-231 (1969). 36. Mekhedov, L. N., Factors participating in alpha-toxin production by Cl. perfringens BP6K in media of known chemical composition. I. Mechanism of the stimulating effect of excess arginine on toxin formation. Zh. Mlkrobiol. 4jK8), 117-124 (1969). 37. Mohs, H. J., Hygiene of deep-frozen foods. Bacteriological investiga tions during manufacture of deep-frozen vegetables. Gordian 69(1630), 374-376 (1969). 38. Mollenhauer, H. P., Food control and food standards for consumer protection in developing countries. Food Drug Cosmet. Law J. 24, 259-267 (1969). 39. Murray, J. G., An approach to bacteriological standards. .J. Appl. Bact. 32, 123-135 (1969). ' DSW 033491 ! T.-?rr mmmj, STLCOPCB4017453 323 40. Neri, M. G., et al., Virulent bacteriophages specific for Pseudomonas aeruginosa. . Microbiol. 1M2/3), 107-114 (1966). 41. Patterson, J. T., Salmonellae in meat and poultry, poultry plant cooling waters and effluents and animal feeding stuffs. J. Appl. Bact. 32, 329-337 (1969). 42. Peeters, H., et. aJL., The isolation of Salmonella with Taylor's medium. T. Gastroent. 12, 79-81 (1969). 43. Prost, E., et. til., The meaning of Clostridium perfringens in food hygiene. Med. Weterynar. 24_, 579-582 (1968). 44. Rappole, C. I.., Sanitary control in on-pre.mise cooking and freezing of food. Cornell Hotel Restaurant Admin. Quarterly 10(2), 13-19 (1969). 45. Ryskina, T. B., On the evaluation of the method of indication of Shigella by means of media containing antibiotics. Lab. Delo. 1, 50-51 (1967). 46. Sainclivier, M., et al., Technics fo`r the bacteriological examination of butter. Ann. Nutr. ^3(3), A27-A38 (1969). 47. Sata, K., Radiation sterilization of medical devices and supplies. 6. Disposable syringes and needles. Eisei Kagaku 15, 22-25 (1969). 48. Schmidt, E. W^, Chemical preservatives to inhibit the growth of Staphylococcus aureus in synthetic cream pies acidified to pH 4.5 to 5.0. Food Technol. 23, 1197-1199 (1969). 49. Schothorst, M. van, Salmonella in dried milk. Neth. Milk Dairy J. - 23, 222-223 (1969). 50. Shimizu, Y., ejt jal., A study on the pearly layer formation of .Clostridium botulinum. Kitesato Arch. Exp. Med. 38(1/4), 87-91 (1965). 51. Smith, R., Maintenance, Sanitation Report. Food Can. 29(8), 33-41, 48 (1969). 5$. SulMvan, R., et, al., Thermal destruction of adenovirus 12 and reovirus 1 and Herpes simplex in milk-. .J. Dairy Sci. 52, 897 (1969). 53. Suzuki, A., et al., A survey on the Salmonella contamination of imported meats during 1965-66. Bull. Nat. Inst. .Hyg. Sci. 85, 188-195 (1967). 54. Ulisko, I. N., et al.. Laboratory diagnosis of Sonne Shigella by the immunofluorescent method. Zh. Mlkrobiol. 45, 14-18 (1968)., DSW 033492 STLCOPCB4017454 3.74 55. Vernon, E., Food poisoning and Salmonella infections in England and Wales. Public Health 83, 203-223 (1969). 56. Vitez, I,, Research regarding the production of anaerobic toxins. I. Clostridium bolulinum toxin type A and type B. Acta Pharm. Hung. 38, 353-360 (1968). " 57. Vitez, I., Research regarding the production of anaerobic toxins. II. Type A Clostridium perfringens toxins. Acta Pnana. Hung. 38, 405-410 (1968). '~ 58. Weissman, M. A., ejt ol., Incidence of Salnonellae in meat and meat products. Appl. Microbiol. 17, 899-902 (1969). 59. Wojton, B., et^ al., Influence of curing salts on the. behavior of Clostridia in canned pasteurized hams stored at various temperatures. Bull. Vet. Inst. Pulawy 12(1-4), 67-68 (1968). / CSW 033493 STLCOPCB4017455 325 Interburcau By-Lines No. 6 May 1970 PUBLICATIONS LIST FOODS, HEALTH Microbiological Contamination Houghtby, G. A., and Kaysner, C. A., Incidence of Clostridium botullmun Type E in Alaskan Salmon. Appl. Microbiol. 18, 950-951 (1969). Chemical Contamination Pesticides 58-70 Biros, F. J., Enhancement of Mass .Spectral Data by Means of a Time Averaging Computer. Anal. Chem. 42, 537-540 (1970). 6-70 Cranmer, M., and Freal, J., Gas Chromatographic Analysis of Pentachlorophenol in Human Urine by Formation of Alkyl Ethers. Life Sci. (Ft. XI) 9, 121-128 (1970). 214-70 Lawrence, Jr H., Barron, R. P., Chen, Jo-Yun T., Lombardo, P., and Benson, W. R., Note on Identification of a Chlordane Metabolite Found in Cheese and Milk. J. Asa. Offic. Anal. Chem. 53, 261-262 (1970). ' Robens, Jane F., Teratogenic Activity of Several Phthalimide Derivatives in the Golden Hamster. Toxicol. Appl. Pharmacol. 16, 24-34 (1970). ' Sphon, J. A., and Damico, J. N., The Mass Spectra of Some Chlorinated Aromatic Pesticidal Compounds. Org. Mass Spectrometry 3. 51-62 (1970). Williams, Clara H., P-Glucuronidase Activity in the Serum and Liver of Rats Treated with Parathion. Toxicol. Appl. Pharmacol. 16, 533-539 (1970). Food and Color Additives 44-70 Chen, Jo-Yun T., Oates, Nancy C., and Firestone, D., 3,5- Dialkyl Phenols and Their Allyl Substitution Products: Infrared Absorption Spectra and Interpretation of Charac teristic Frequency Shifts. .J. Ass. Offic. Anal. Chem. 53, 275-287 (1970). DSW 033494 J*.| I WJ <mn '*<w -------ry i i STLCOPCB4017456 73-70 Hobin, Nancy K., Turbidimetric Determination of Soluble Sulfates in Water-Soluble Color Additives. J. Ass. Offic. Anal. Chera. 53, 242-243 (1970). 89-70 Howard, J. W., Fazio, T., and Watts, J. 0., Extraction and Gas Chromatographic Determination of N-Nitrosodinethylamir.e in Smoked Fish: Application to Smoked Nitrite-Treated Chub. J. Ass. Offic. Anal. Chero. 53, 269-274 (1970). 7-70 Legator, M. S., Mutagenic Effects of Environmental Intrusions. Quart. Bull. AFDOUS 34(1). 3-5 (1970). Mayer, V. W., and Legator, M. S'., Induction by N-Methyl-N'nitro-N-nitrosoguanidine and UV Light of Petite Mutants in Aerobically and Anaerobically Cultivated Saccharomyces cerevisiae. Mutation Res. 9, 193-198 (1970). 68-70 72-70 Seward, C. R., Mitchell, G. Vaughan, Argrett, Loretta C., and Hove, E. L., Oxidation of o?-Tocopherol to o-Tocopherylquinone by Carbon Tetrachloride-Ethanol Solvent. Lipids 4, 629-630 (1969). , Singh, Manjeet, Determination of S^'-Disulfo-S^'-dio^o-A^' biindoline, Disodiura Salt, and 5-Sulfo-3,3*-dioxo-A^^ biindoline, Sodium Salt, in FD&C Blue No. 2. J. Ass. Offic. Anal. Chem. 53, 250-251 (1970). % _. * Stein, C., Determination of 2-t(2-Hydroxy-l-naphthyl)zo3-6- naphthalenesulfonic Acid in D&C Red Nos. 10, 11, 12, and 13. h As5_. Ctea, 240-241 (1970). Natural Poisons Armbrecht, B. H., Shalkop, W. T., Rollins, L. D., Pohland, A. E., and Stoloff, L., Acute Toxicity of Aflatoxin Bi in Wethers. Nature 225, 1062-1063 (1970). Drug Residues Lakata, G. D., Methods Evaluation in the Chemical Analysis of Drugs in Animal Tissues. J. Ass. Offic. Anal. Chem. 53, 224-226 (1970). 78-70 Wright, W. W., Detection of Antibiotics in Animal Tissues. J. Ass. Offic. Anal. Chem. 53, 219-223 (1970). Other Health Hazards Levander, 0. A., Young, M. L., and Meeks, S. A., Studies on the Binding of Selenium by Liver Homogenates from Rats Fed Diets Containing Either Casein or Casein Plus Linseed Oil Meal. Toxicol. Appl. Pharmacol. 16, 79-87 (1970). " DSW 033495 i .... ...... .................... -- -- a- rr'^nrxjmrr STLCOPCB4017457 * 327 Robens, Jane F., Teratogenic Effects of Hypervitaminosis A in the Hamster and the Guinea Pig. Toxicol. Appl. Pharmaco]. 16, 88-99 (1970). '" DRUGS Hazards 63-70 Alieva, J. J., Waleski, Mary V., and Alieva, F. R., The Zeitgeber for Ovulation in Rats; Non-Participation of the Pineal Gland. Life Scl. 9(Pt I), 241-246 (1970). 50-70 Brunner, Charlotte A., and Kunze, Frieda M., Analysis of Mestranol in Combination with Norethindrone or Norethynodrel by Partition Chromatography and UV Measurement. .J. Ass. Offic. Anal. Chem. 53, 234-237 (1970). 5-70 Quaife, Mary L., and Friedman, .Leonard, Failure of the Vitamin E-deficient Rat to Show Decreased Liver Codeine-O-demethylase Activity. Prnc. Soc. Exp. Biol. Med. 133, 849-852 (1970). Wojtowicz, E. J., A Column Chromatographic Method for the Determination of Sulfanilamide in Pharmaceutical Preparations Containing Sulfacetamide or Its Sodium Salt. J_. Pharm. Sci. 59, 240-241 (1970). Yen, Helen C. Y., Krop, S., Mendez, Halina C., and Katz, M. H., Effect of Some Psycho-active Drugs on Experimental "Neurotic" (Conflict-Induced) Behavior in Cats. Pharmacology 3. 32-40 (1970). HAZARDOUS SUBSTANCES ' Brown, D. J.f Determination of Ethylene Oxide and Ethylene Chlorohydrin in Plastic and Rubber Surgical Equipment Sterilized with Ethylene Oxide. J_. Ass. Offic. Anal. Chem. 53, 263-267 (1970). LABORATORY TECHNIQUES ' Jaffee, M., and Ford, L. A., On the Nature of Quenching. Intern. J. Appl. Radiation Isotopes 21, 49-32 (1970). i& i ! --TT nr * OSW 033496 STLCOPCB4017458 CUMULATIVE INDEX TO INTERBUREAU BY-LINES VOLS l-6! Abrnmoff, J., p`.(*iylov'rcurlc ace: ico In complex drug* by ulnfllp-nvvpp polnrogrnphy, 2*271 application ot the A"AC conjugated estrogen method to eon- pier creamo, jhlDl (corr. 2*150) mtlunl 11 Jgr.ir- quantities of atropine sulfate In single tablet* jtviI cct'i'o* 1 tea, 2.s93 Aei toolltill*, Irpurity in, 6:23*3* Arc! y}--ftl Uoj k nvl sull.mil/ir.ldc, In medicated feeds, 2*267 Adulteration, vefi l,.SIc fot In butter, 6:19 Allot oxins, dcconLic,ilrioticu procedure, 1:263 Sue ;dW Mviouu-.tnft A1 coho'] t, "by ol C, ?.;2U AJdrtn-dieldrln teoiduos, in sugar beets, 2:217, 3:91* Alt/.mdur, T. C., analysis of LSD preparations, 2:149 (cocr. 3:32) * uiway of ly.fte>bie add nmldes In morning glory seed, 1^67 S'l-p nlao Koch, S. A. AIIu'.w.uin7 In ikrti.uolcglc preparation::, A_;5? Aclracrino, fluuror.vtric assay, 2:85 /u.VMUiiA, Index of crib: .>.*( decomposition. *.2B1 Amphetamine, assay of mixtures with other drug*, 4:279 Amplifiers, In laboratory instrumentation, 6:119 Andrus, C. N. , and Snow, S, W., LTV absorption data Of pharmaceutical*, 4.: 121 Andrew, M. L., collaborative study of grlscofulvin particle alto, 1124.5 ' Anesthetic gases, analysis, 2*11 Antibiotics, fishing tcchnlquts, :79 assay of steroids In, interferences, 1:279 neomycin-hydrocortisone mixtures, 2:209 non-sttrlle, Rsaudorncpae asrualnosa in, .5:157 penicillin contamination, :49 procaine penicillin In feeds. lt$7 sterility tasting, 3:1 Antihistamines, column chromatography, 6:85 Tl.C, 5:171 . ** Arorlor*"l254 and 1260, behavioral studies, 6:313 Atsonic, In swine liver tissues, 2:165 total diet samples, 1:251 Ascorbic acid, and the common cold, bibliography, 5:229 oxhIIc acid contamination, 3:85 AnMng techniques, antibiotics, 6:79 Atomic absorption, vitamin B assay, :23 Atroplns sulfate, tablets ana composites, 2:93 Authentic data, cheese, ahclokage, 1*9, 1:15, U26, 2l95, 2t96, 2:98, 2:100 . ~~ ~ ~ Concord grape juice, 2:137 (corr. 2:94) crabaeat, drained weight, 2*259 cranbarrles, 4:67 prunes, 2:1037 4:141 rsspberrlas and strawberries, 4:61 Automated analysis, coaputor-asalstad, 5^:73 Automated Injection syacats, CLC, 6157 Automation, at the National Canter for Drug Analysis, $\M microbiological assays, 6:31 ~~ Availability, drugs, tharapeutlc equivalency, 5:11 Bacterial contamination, Salmonella In frog log's, J5:69 Bacterial growth In mouthwash containing preservative, 6,* 169 Bacterial studlep, mlcto-sllde gtl-diffusion east, S:247~ motility teat, 5:241 " ptcparstloQ of froten vagatablaa, :189 Dakicli, N. , and Cull, G., experiences with analysis of I,$n aat:pleu, 4:119 Banes, D., scientific evidence in court ceatlmony, 3:185 soma scientific ospeccs of the Krebloien caso, 2:245 Barbiturates, by CLC, 1:203 " Sarcklow, f. c., and Ssymanpki, H. A., Identification of commercial trlethylenntutramlne and tciratthyleno- pcntatninc by TLC and NKR spectroscopy, 3.:163 Barry, T. L., eeu Bellman, S. W. " Beaver, L. A., soe McNerney, F. C. Behavior Studies, DDT, Aroclor 1256, and Aroclor 1260, in rats, 6:313 Bellman, S. W,, subaicregratn quantities of Iodine In vieamln- olnernl preparations by oscillopolarography, 2:229 (corr. 2:270) " Sec also Kraw, T. C. Bellman, S. W., and Berry, T. L., combined CLC-tsaaa spectrometry, 6:182 Bellman, S. W, , Tutctan, J. W., Ileagy, 3,, and Hopes, T. H., structure elucidation of 5:113 (corr. 5^:170) Benaon, w. R., and Jones, K. A., chemical literature of pesti cides, 2*55 Benzoic acid, Tn Whitfield's ointment, 2*153 Derturri, p, K., extraction of chlorinated pesticides from samplcR of low moisture content grains and feed*/ 3^i 27 Bethea, S., and Hllllg, 7,, determination of trinethylaolnt nitrogen In extracts and In volatile fractions of flah. 2?153 Bayer, E. see Hat tin, R, J. Beyer, 2., and Dachert, D. D. .,identification of LSD and LSD tartrate by TLC, ;21 Blanch!, R., see Rosensteln, .T. Blanchl, R., and Gruenfald, H , Identification of patrol#** distillates, 6^:9 Bibliography, ascorbic acid aid the common cold, 2*229 column trap chromatography, .3:57 cyclaoates, 6:43, 6^:99 ~ drug information aids, 3:5 Iron In nutrition, 2*251 microbial'contamination, 6:229, 6:320 mycotoxins, 3:95, 3:134, 3:193, 3:241, 4tl33, 4:203, 4:237, .4*297, 5:92, 5:135, 5:377, 5:220, 5:271, 6:36 ~ neutron activation analysis, food products, 6:194 pesticide -Aformatloo aids, 2:35 ~ qustarner, amaonium compounds in food, 6:263 steroidr, 6:161 ~ Blossssy of*LSD, with fish, .3:201 Blakely, J., and Seleer, C., determination of tulflaoxasola and acetylaulflsoxasola by Bratton-Marshall method, :127 Blomqulac, V. H., sea Boland, f. E.; Verran, J C. ** Btooqulac, V, H., and Dads, W. W., relation between percent by weight of rat and Howard mold count In cominuted large fruit products, 2*213 Boland, t. E., Rlomquiet, V. H., and Bstrln, B., chemical com position of fresh cranberries, 4:64 chemical composition ot fruits, 2:61~ Bond, J., ass Duggan, B. ~ Bowman, t, W., atarlllty taatlug of antibiotics, 3tl Bowman, F. W., and Knoll, E. W,, laminar flow tor environ mental control and starlllty tasting, 3:110 Hhe Index for Volume 6 is Ineludsd in the cumulative index; no separate Index will be printed. DSW 033497 STLCOPCB40 A., W.ivlutid, L. C., Kantor, N. H., and Welr.B, p. J., ub*txnrcf that Interfere with a*;H*y of curtlcoatcroHa In antibiotic pivp^ratlom, 1:7.79 ,1 ,-mon, W I,, in* ;-.('naive improvis'd IK p.jA coJJ, ico also Haydun, A# L.; Uaiiiuul, u. /in. v*r , J. F., w*ic Di-'J, H. L. ji .K-vlonl, J. cVr*ui ilysla and tdroll f I cation of dimethyl* Iryplarcinc, 115 Huhr, C. A., cvaluoTittg data of multiple samples fro* a nlngio dmp, code, 6^5157 IHrke, J., pcaMcldt-s in human ni)k and tissue, 2:205 Hti'.ttT, vefielablu fm adulteration, 6:1V Ivton, W. R., y-< < f'Jix.'f, A. L., Jr. C.'.Jiuium. in icoJ.-.tot (s , po l*ioprophyf ^: i02 j;*)c 1 iiu Nulfote, u-J-iurWfil lui Tl.C, .1:^37 C.'tihnun, H. P.. t.n.f hUlory of aeruginosa in non- atarlio antibiotic product*, 3:157 Ciupbcll, E. J., evaluation of Barbor-Colraan automatic injec tion aypte'n, C:5? Carharflono, ftt food*, .2:237 C.'irOtnoxomlno, GhC, 7.; 117 Carcinogenicity, testing color additives by mouse-akin painting, 5:105 Carol, J., genetic equivalency, JS1113 recent progress in thyroid assay research, 5:125 39 years of clungp n* aeon from withli. >1>A, :247 Carotenoids, in shrimp, 2:lfl9 Carson, N. A., medicinal' uat analysis, 3:119 Gasmen, E. P-. micro-slide. gel-diffusion detection of staphylococcal cnterotoxlns in food, :247 Csatcrline, J. L., Jr., sec Williams, C. H. Cvloste, A. C. Polito, M. V. Cell biology, genetic effects of chemicals, J^i 133 genetics, ,2:233 Cereal products, filth, 3:313 noodles, sterols as cholesterol, 4^:229 white mineral oil in, 2:291 Chock sample program, FDA tegulatory laboratories, 3:69 Cheese, packaged, shrinkage studies, 1:9 (corr> 1:146), 1:15, 1:26, 2:95, 2:96, 2:98, 7:100, 2,i107 orbi" acid assay, 2:81 Chloral hydrate, chloTnbencen* contaminants, ,1:297 Chlorinated cleansers, in milk, 2^31 Cidorphaniramina, in cembinatiofTwitb other cold preparations, 3:8) Chloroform la liniment, polarography, 161 Chocolate, estimating shell In, 4:39 Cholesterol, atevola in egg noodlae, 4.:229 Choltnsstersia, toxicity of Band to rats, 4,: 177 Chu, R. C. L., aeaay of aHantoin in dermatologic preparations, 4:57 Clark, E. C., analytical usaa of near IR spectroacopy, 6,:116 spectrofluorometrlc determination of Rauwolfla serpentina, tablets and whole root, 6:289 Cold preparations, analysis, 2*61 Color additives, in food, paper electrophoresis, 1.J225 mouse-aklQ painting study, 3:105 trip electrophoresis, 1j227 UV spectra, 6:192 Computerization, automated analysis, ,5:73 ` drug methods retrieval, 3:207 ' glassware procurement and Inventory control, 3^33 NMR literature retrieval, 4:269 publication procurement, 5:215 Confectionary analysis, mineral oil on hard dandy, 3:47 suearyl, 2^3 Confectionary manufacturing, analytiesl entomology, 189 Cornellussen, P. E, see Rampa, L. R. Cornallusssa, P, E., and Ramps, U R., fate of aldrln-dleldrln residuae In auger beat processing, 3:91 Cornett, E. W., TLC method for rodent urine contamination, 2^:235 Corticosteroids, decomposition analysis, :151 TLC eeperetlon and roactioo with sulfuric acid, 5.1? Cosmetics, <LC of propel louth, 1_:219 raowsu-J-'kin pointing studv, 105 tion< lrv mu, b.irtrr jnl yrow(h In, : 16 9 Cuunterieit dru?., barbiturates uud Amphetamine*, lUetic: lien* txC't' of r aivu yctui''*-, CrabBc.it, Armenia as Index oi decomposition, 6:231 frozen, duincd weight, 3:2-9 Crnckers, filled, packuRod, shrinkage study, 2^:227 Craig, N K., i'k( r.iccioit apparatus tor quontl tat ivo Isolation of compounds frc-r. thin layer chromatograms, 2:143 Crawford, K. M., see Major, A., Jr. Cull, C., sou Bakich, H. Cushtsac, H-i see Rodrlcks, J. V. CyclanatcH, bibliography, 6:43, 6:99 Dada, V. W. , pee Hlooiquiut, V, ll. Dairy products, tr.anure In, 1:77 Damaaka, W. M., TJX: detection of chlorinated pcsilcides, pruvnehing of adsorbent, addition of silver nitrate, 1:85 Damico, J. N., muss spectronetry: some practlcnl applications to current probleeis In Division of Food Chemistry, 1^:28 7 DDT, effect on central nervous system, 6:313 Dechert, D. l>., method for drying apactrophotomctric cvll, 1:83 rapid identification test kit Cor materials containing ergot- type alkaloids, 4^17 See also Beyer, E.} Martin, A. J. Dechert, D, D., and Jekabsone, E., LSD analycla, 4:31 Decomposition, crabmeet, aoimoitla as an Index of, 6:381 fish, 1:153 " fish, organoleptic examination techniques, 5:121 nitroglycerin, with sagneeluo oxide, 4.:193 shrimp, carotenoid pigments, 2:189 organoleptic and chemical Indices, 6:304 Decontaninatton, *flatoxins, 1:243 DarmatoLoglc preparations, allantoin In, 4^:57 Dexbronphenlranine, in cotnblnoctoo with other cold preparations, 2:81 DeZan, P,, optical rotary dispersion and Its applications, 5^81 Diaz, R., aee Zeeberg, 8. Diazepam, decoapoaitlon product, 3:161 ~ Dlchlorobenzeno, contaminant in chloral hydrate, 1:297 Dick, R., responsibilities of Food and Drug Adalniatration under Tea Act, 317 Dieldrin-aldrin residues, sugir beets, 2i2l7t 3:91 Dleldrln, residues, carrote, 2:263 ~ Dlethyleellbeetrol, io animal feeds, polarography, 1^307 Dlgltoxln and dlgoxln, gltoxin in, 6:25 Dilodohydroxyquln, UV and IR spectroscopy, 6:179 Diaethylaulfoxlde, by CLC, 2^:279 H,N-Dlnethyl tryptaalns, and lnteraadiataa, identification, 3:27 identification by TLC, 2:H.5 3,5-Dlnltrobensa0lde in medicated feeds, 2:267 in poultry tissue, 4:75 Dithiocerbamates, acid hydrolysis method, 1:255 chemistry of, 2:177 DMT, see N,N-Diioethyl tryptamine DNRA, ace 3,5-Dlnltrobeuzamlde Doherty, J., radionetrlc method for meaaureaonc of acetylcho linesterase activity In rat blood, 4^:85 Dollmpio, D., see Legator, H. Douglas, C. C., GLC analysis of phenols combined with other substances, 2:21 Dow, K. L. evaluation of tablet pulvarlzsra for drug sample preparation, 4:197 Dow, M. L., Rlrchhoefer, R. D., and Brower, J. F., rapid identification And eetlmation of gltoxlo in dlgltoxln and digoxln tablets by. TLC, 6^:23 Drug abua^, amphetamines end berbituratea, identification of manufacturer, 3:12 7 Control act, 3:113 osw o33`,9S STLCOPCB4017460 > Dr*i ./aaJvyltf, automation, 'it 37 1-,'|i;::i trap clrom-it.<.T ip'v--, hi V 1 ioj;r.irhy , JtW bin,. A:,.|^v` C^.-.troi Act, j:Ki I v!r;ClIun technique, 5:1* < r ( Iv'-l V i (. , ;*;L7 f: ii--rvt'c t ry, 6:135 ioforiaiion retrieval, .5:207 I r.forr-.at u-nil Aids, 3:3 j p -r ;t r 's<*tpy, 1; 3 r.foMori*n c.ah*:, 2:2*3 h-'ur l`.i spectroscopy, 6: lib LMh, 0:237 mniMij'icouu titration tvehn I queh , 5.: 125 rotary di?;*"r'lcn, 5?#). pJU manufacturer Identification, 3:127 polarography, :1 ctottsiiJCjJ concepts, 6:157 sterility trr.tlnfc, 6:00 tablet pulvor I cuv*, 4:197 TIC on poroua glaAR, :61 t'V spectroscopy, data compilation, 4:121 X-ray fluoroaownce, 6:140 Drug residues in animal tlv.nues, areenlc In awino liver, :165 3,5-dlnJ vrobtnzamidv In poultry, 75 Drugs, allontoin, 4:57 aulnocrinc, ^:85 an.pheiarai.ne, ;279 antifungal preparations, 5:279 antihistamines by column chromatography, 6_:83 by Tl.C, 5:171 atropine eulfata, 7:93 barbiturates, by 01C, 1_:203 carbinoxaralnc, by CLC, 2^4117 ^hloroforn in liniment, :161 cold preparation, 2!&l conjugated estrogen*, 6:145 contaminants In chloral hydrate, ^:297 corticosteroid#, ^:279, 5:7, tl51 counterfeit, identification, .4:95 diazepam decomposition product, .3:161 dliodehydroKyqum, 6:179 NN-dl&iethyl tryptomlne, 2:115, 5:27 etrogene, 1^101, 3:225 generic equTvalcncy, :113 glcoxin In dlgitoxin and dlgoxln tablets, 6:25 1 gold sodium thiosulfate injcctsbles, *.103 griaeofulvin particle cite, 1^:245 hexachlorophene and resorcinol, 1:105 hext*trol and phenobarbital, 1:201 iron, 2:241 ~ LW, 5:113 (corr, 5:170) LSD, 21149 (corr. 3:32), 2:153, 4:3, ilO. 4:15, 6:16, 4:31, 4:U9, 5:201 " by 1R, JillS, 4:2*, 4:26 by paper chromatography, 4:19 by TLC, 4:21 " field teat, ^3:177 lyoergic acid amide*, 1:87 vodiclnal gate*, 3:119 menadione #odium bisulfate, 5^:285 mathonealnc, 2t109 2-sethyl-3,4-nethyl*nedloxypbnethylamine, 4:271 neomycift-hydrococtlavne mixture, 1.1209 nitrates by palaeography, 6:299 nitroglycerin, 4:193 nomenclature, 2^07 ophthalmic preparatlone, 6:113 oxtriphylline end theophylline by TLC, 2*159 peyote identification, :29 * phenols in combinations, 2:21 phenylephrine in ophthalmic preparatlone, 4:113 phenylmercurlc acetate by polarography, :57l paiiocybin, itlQ7 Drugs (continued) pyridoxlne IU; 1 and meclizine ifCl, 2:183 qcinwer J i'f hviJrochloride, : 255 f;uinldme tuilfnte contamination, 6:237 Fhvvr..;0.!/.! u t tna by f lu^rortetry, b: 24*6 #f.jbjlir>, 3: 2 3 steroids, 1:269, 4:35 Abstracted bibliocfCphy. 6;J61 iju1 far.-thivh.e in feeds containing procaine penicillin, 1:197 ctil 11? *: A/ole ard ncctylsulfisoxazoic, 127 Fyrjp;tt`cr<ia:^c I cs , 4)261, 4:275 thallium by polaroe.raphy, 2:11 themp'.utie. availability, 5:11 thyroid ttSfiay, J1;125 Whitfield's olntmunt, 2.: 155 Duggan, B, , and Kond, J., CLC profile* of sugars occurring in natural products, 4:147 Dye extraction technique, phnrv.oeeut 1 cal analysis, 5.: 15 Edge, J, drug analytical irethndu retrieval, 5:207 Egg content, analytical constants in food, 2*33 F.ggs, incubator reject, :59 (corr. 1:146) Egli, K, L., physiological effect* of d-lyserglc ncld diethyl amide. tartrate on Butt* splcndens (Siamese fighting fl#h) and Lcbistcs retlculatua (guppies), 5)201 EJduoon, 11. P., KDA Institute for Advanced Analytical Chemistry, 3:295 Electrophoresis, disc, differentiation of neat specie#, 2:131 fish species identification, 1^:81 paper, for color additives, in food, X^:225 strip, color additives, l.:227 Emission spectroscopy, applications, 2^:269 * Eudelaian, A., statistical background for sample site formula, 2:35 (corr. 2:114) Endrin residues, effect of processing of carrots, 1^:203 F.nzymc analysis, acetylcholinesterase, 4:85 Enzyme#, chollocaterate mtasurement of Banol toxicity, 4:177 Equipment check programs, FDA regulatory laboratories, 3:69 Erickson, J. V,, bacterial growth In mouthwash containing preservative, 6^: 16^ destruction of Salmonella in frog legs during cooking, 5:69 Erney, D, R., steroid analysis by CLC, :269 Eatrln, B., ace Boland, T, E. Estrogens, colorimetric aeeay, V.ll*) conjugated, 6:145 In complex crooas, 1:101 Estrone, with progesterone and testostarone, 4:35 Everett, R. L., screening method for rodenticldc# In bolt eamples, 4:51 Experimental data, line of best fit, i247 Fatty acids, in vegetable oil#, unusual oil#, marine oils, margarine#, 2:5 Ftede, acetyl--nltrophenyl aulfanlUmlda and 3,5-dlnitrobenaamido In, 2;267 carbareone In, .2:237 dlethyetilbeetrol in, l.:307 nltrofurazone and furaeolidone In, l,:15l 3-nitro-4-hydroxyphenylareonic acid contaminant, 4:285 Sodlua ^-asiinobanBoate Interference in aulfaaethazlue assay, 2:91 sulfamethazine and procaine penicillin In, :97 (corr. 2:92) Fehrlngcr, N. V., analysis of mono- and diehlorobenfette contami nants in chloral hydrate solution and capsules, :297 TLC using microscope slides as plates, 1:197 Fein, A., see Roaensteln, J. "" Femander-Floraef E., modified method for separate determination of nltrofurazone and furazolidone in feed, 1:151 See alen Prochaxka, H, ~ Fig paste. Insect filth In, 2:39, 2:45, 4:223 Filth, baked goods and alimentary pastes, 3X3 lnsecu in fig paste, _2:39, 2:45, :223 manure. In dairy products, .1:77 rodent urine, TLC, ^:235 DSW 033499 STLCOPCB4017461 nnoccblQTo, j. N. , dlthit-c.-irhannU**, 2:1)7 Mnetcrvalder, C. K., chlorinated compounds in milk due to K} censor* , .2: 31 Ffah, uu fern nipiriis'i for LSD, 5:201 or.,hr`.if, WccT.hc/...ii*n, 6:2di drained weight, 3:2^9 dcci'&poail Jotl, lrIxi'lhyl wiinc, 153 '.''vTiHury <-*n,nln.t ion of drconmoBi tion odor*, 5:12J r"\-:<vln concentrate, Isoprop.anoi in, A: 71 vl.ri^p, carotenoid pi^menta, 2:i69 organoleptic and chemical Indict* of decomposition, 6: 3CV* prelr-s Identification, J.:6l " ouukerel, 5:53 snipper, 5:153 \wjt pyrophOMplmie In, 3:6? Mtr.porald, J. V. , bibliography on quaternary ammonium cob- pounds in fond1-, !; T#>3 Fla,iie pbot'.'mottr, propatiition for use, 1:163 Fluoride*, In Bolder fiu^es, specific fluoride electrode, 6:225 Fluoroc'ctric analysis, mtlnacrine in drugs, .2:65 diuge, 6:135 quinserlno hydrochloride, M 255 quinidlno sulfate aa contamination, 6:237 Rauwolfl* serpentina. ;208 atomic* in uga noodles, 4:229 Food additives, 1,5-UNUA In poultry tiaaue, 4:75 formaldehyde, 5.:263 isopropyl alcohol in fjeh protein concentrate, :7l mineral oil on hard candy, .3:47 mineral oil (whito) in bokory products, :297 rubber materials extractives, 2:63 sorbitol by CLC, 3:169 Food and Drug Administration, early problems, .1:167 Institute for Advancod Analytical Chemistry, 3:295 new laboratory building, .2:147, .2:201 39 yoatl of change, 6:247 Formaldehyde, in foods, by colorimetry, 5^;283 Frasch, D. L., sea Manak.e, D. D. Fretnan, C, C., mackerel or Jack cscksral?, 5.:51 Friu, J, C., iron In nutrition: stlected references vith . annotation*, 15:251 t Frog legs, Salmonella in, 5:69 -V Fox, R,, identification and determination of o--sethyl-3,4- nethylenadloxyphenethylaalna, 271 Fricko, F. L., determination of dlmethyltulfoxlde by GLC, 2:279 Frickn, F, L., and Xeppel, G. ., Isolation and identification of aucaryl In .dietary. caMy end chewing gum, 3t23 FrladnAn, H., aeo Tanner, J, T. e Fruit, chomlcaF composition, 4:61 comminuted, rot and Howard mold count, ^)213 Concord grape juice, 2:137 (corr. 3:94) et-anberrleacheaicsi compositor*, 4.67 drinks, tin and iron In, .1:14? fig psnie, insect filth In, 2:39, 2:45 fig#, filth in, 4:223 "" prunes, 2jl83, :141 Fry, B. ., Jr., datsroinatlon of lino of best fit (least- aquarea) for curvilinear data, 4.: 24 7 Furacolldone, In fsad, l_i 151 Cajan, R. J, polarographlc determination of eadmlta in foodstuffs, 4:107 Sea also Prochatka, M. Oaa call, lnfrarad, contamination, i291 (prevised 2<303 " . Gas chromatography, alcohols, 2:221 aldtln-dioldrio raalduea, 3:91 barbiturates, JL1203 carbinoKAAine, 2tll? cleaning of alsctron capture trltiw aoutca, 4.170 column for pesticide analysis, 2:71 dlmcthyisulfoxide, 2:279 iaopropyl alcohol in fish protein concentrate, k\1l mothanamins, 2*209 ilk, chlorinated claanaara in, 31 U.'< f'hmi.niHnT.Vfhy (i nu\ )nu**d> rplic.-tl Isoyn-ra of .sytnpntho!nfnrti.c amine*. 4:275 pesticides automatic inK'ctluii Kyatem, 6:57 Jr. ni Ik m.-J 2:205 pt'l r. l-.-r.! ili :*:). ;,t, i-:V phenols In pharmaceutical cor.hin.'.i ion#, 2:21 j):vpcllcTil:i hi coyiin.'tIc8 , l:J9 mpacacirm of solvent mixture*, 6:175 sorb 110), 3:169 steroids, J_:2''9 sugars in natural products, 4:147 Teflon heat shields for infection diaphr*cm, 1:36 trace amounts of trlehlorobcnzony in foods, .5:195 vegetable fut adulteration In bu'.tcr, 6:1') xylene and toluene paint thinners, .2:195, Gs chromatogropfy-Dio58 speccremrtry, 6:132 (corr. 4:222) Cases, medicinal, 3:119 Gecsn, J. S., analytical entomology of confectionary manu facturing, ji: 169 Cel-diffusion, utnphviococcfll entorotox Ins, 5:247 Cenerlc equivalency of drugs, 6:113 Ceuotlcs, cell biology, 2:253 effects of chomlcals, f:l3J Cerrlts, H. W.t effect of processing on endrin and dloldrln residue content of carrots, .1:263 Giles, A. L., Jr., and Byron, W. R., mouie-skln painting study Of 2 colors and several cosmetlcal Ingredients compared with DKBA, _5il0S Cltoxln, TLC with dlgltoxin and digoxin, 6:25 Gluffrlda, L., cleaning lnatructlona for electron capture tritium source, ,4:70 Giuffrtda, L, end Ivca, N. F., ImpTOvementa for GLC column uaed for peuticlde analysia, 2_t7L . Glass, porous, or TLC adsorbent, 5:6) Glassware procurement and inventory control, automated, .5:33 Gold sodium thiosulfate, polarography, 4^:103 Goldhamaer, C. S., the expert witness IV, case of incubator *88 1*59 (corr. 1^146) Goldstein, B. P., see Nleleen, J* K. Goldstein, H., detection of mineral oil 00 hard ctndy, 3:47 Coldston, B. R., ace Stakelua, G. S. Graham, J, K., colorimetric asuay of natural estrogens, 2:*25 Grahsa, R. E. selected abetra:ted bibliography on steroids, 6:161 special problem in corticosteroid decomposition analysia, 6:151 Graham,A., separation and identification of color additives In foods by paper electrophoresis, .1:225 Crains, chlorinated pesticides in, extraction of low-moisture samplee, 3:27 lead In, by polarography, 2:213 Grant, R. C., Scheme for rapid aeparatlon and identification of antihistamines by TLC, 5/.171 TLC of soae sympathomimetic*, 4^:261 TLC separation and identification of some corticostaroida by their reaction with sulfuric acid, 5:7 Green, S., sec Legator, K. Crotch, F, H., identification of N,H-dlmethyl tryptamlne and Its intermediates, 5^:27 Grimoett, J, A., dlfferentletlon of species of meat by disc eiectxophoie&is, Crlaeofulvtu, particle sice, 1:245 Gross, F. C., CLC analysis of propellents lo cosmetic serosols, 1^: 219 Gruenfeld, M. snalysis of hscsrdous substances, 6:1 analysis of some aromatic hydrocorbons, alkyl and aryl halides sod alcohols in crude staples by NHX, 4^: 157 Infrared gas cell contamination due to sorption of gaskets, .4:291 NMR sptetrs of some commercial turpentine* end theit datefalnatlon, 4:69 separation of gome solvent mixtures on sevaraL GlC columns, 6:175 Saa alto Blanch!, R. /gwigrj';' DSW 033500 STLCOPCB4 rr. t-rv'.'nfvhl, H. nr.J A, F., kerosene In wood stein, 3:223 t urpont i nit! V:t :i-r m 1 'if ui'nu.1 I on ...n J ifi*;owcd ;-.<! ti-nj.; ef infrnrod nnolysls, drugs, 1:3 gun ct.: ] eoiKarninjtiun, 4:291 detor-n.' uaC i r, .1: /vlcrm and t'lucM* in viscous paints nnd i*r. 11 ut product.1;, improvised gas cell, 3:103 ' 3:219 (corr. i:.'!.*'/) rm.demon, K. [.., .v.>(hci.t I c data on prune Juice concentrate .'.nd dried prune composition, : t b3 r :.: /;: : alcohols In riven! laonous products*. 2:221 : . i . J . R. , :* Kc'v. 5*, M. F. , V, J., V.V > ij-r. A., Jr. I > l: *'i.^nns, F, :: d I'n. i h/1 trypt-mil nc and It* Intern,cdlntus, ^lcropoLAKUluo hnllde tlnte technique, 2:285 (cocr. 2.:22) n-illI-,*Ic li.vmtl reflectance, 4^:211 nenr. an.ilyt ical uses, 6:116 undi'cylei.lc acid and aalta in antifonRil preparation*, 5:279 Iodine, lri vltn.T.Ini!, by polurography, _2 :229 (corr. 2:270) Iron, in drugs, ^:241 In fruit drink#, 1^:147 5:27 in autrltion, annotated bibliography, 5:251 hv TI.C, 7:1* IsovphodrJne, in combination with other cold preparation*, 3:81 alUM r:U3 f:149(..-iv. J: U 3 *" 7 :1j J, 4:13, _4 :119 Isopropyl olcnhnl in fieh juotcin concentrate, 4:71 Iverson, y>. L., tatty acid rontenc of vegetable oils, unusual oils, marine oils, and margnrinco, 2:5 bafVgn/u.i'lJ ii C. v.mI J , 4_:3, 4.:10, 4:15, 4_:16 ( Kid tort. , > 77 Ives, N. F.f sjse Gluffrlda, 1., . Jackson, ft. M., review and connentary on method* used to esti I; *t l1 or- o 5 : *'f;i mate chcll in chocolate products, 4:39 lnfriM-rf, }: 2.'`, 4:26 James, T., Kpectrophotofluorometry, useful tool In drug analysis, pi.pcr r npi.v , 4*19 6:133 rbia layer eh* vv * or.r:1, hy. .4:21 Jvsorgir. ucLd m.-.i }'; in wornlnf, glory need*, .1:87 Jeffus, M. T., spcctrophotoaetrlc dettralnatlon of nicotinamide in multivitamin preparations, .1:235 .:-r.ect*yi- J, * h : 2 /1 t '-\yli- ^fct)]xyi>hnt*i h>*l..-iJ no, identification, Jakabsouf, E., see DacharC, D. p. Joe, F. L., Jr., determination of Isopropyl alcohol In fish prvMt, ldchtlficfcUon, 4:29 p-jilocyblii, Idt'-ti f i rot Ion nnd quantitation, protein concentrate using modified Todd procedure, j4:71 determination of whits mineral oil In bakery products, 2:297 itst kit tor ype alkaloids, :)7 See also Whitley, V. P. Karp, A., see l.ejjalur, M. * Johnson, R. l).t spectrophotomatric dotermlnatlon of mensdlons Il'jydcn, A. L., P_Cv K.t'j.u), 0. R. sodium bisulfite In various dosage fores, 5:285 Vi.v.'dcn, A. L., and In cinoon, W, L., ir.icro-pocassiua halide plate Jones, H. A., see. Benson, W. R. technique, 2:?Lj (com. 3:22) Jones, 8. W. , WlHla, J. B., and Libby. D. A., Increasing eha Uor.ardcua aubsiHnocs, coo.l'Jned GLC-mass spectrometry, :182 scope and reliability of the chsaical vitamin D method ruldoliney fur ar.tlysi*, 6:1 * (USP XVII), 2:1 kucuHene in wood ct/iin, 3^:223 Kagan, B., brief view of organophoaphata chamlatry, 2^:103 , WiK of toxic hnJventn, $:157 Kaliman, B. J., see Van Valin, C. C. petroleum dlsuillaifi*, by ClC, 19 Katalnekl, J,, spectra of colors, 6:192 sparotlon ol advent mixtures by Gi.C, :1?5 Kemps, L. R., see Cornellusssn, F. X. solder fluxes, fluorides in, 6:225 Kemps, L. R., and Cornellusten, P. E., location of aldrln- trletUyiene-t<trapine nnd tetreothylcne-pentamina, ^3.1163 dieldrln rasldusa li sugar bests and residue analysis of turpentine, 3.: 2 :>;), 4:89 adhering soil, V.211 vJr.eoaicy, 31 .i Kaator, H. M, see Brscey, A. i xylene nnd (oluer.e in points, 21:195, 3^:219 (corr. 4*222) Xeppel, C. E, modified acid hydrolysis method for dlthlocir- J., ti(-\l.ior>, 9. W. bamate fungicide residues, 1^:255 lulus, K. S., Jr., ace Vstllngton, . M. See aIso trlcke, F, L. )*{Aaehiur<'fOi*rtf? arid trt\?rtlnol In presence of parebena, .1:105 Kerosene In wood stain, 1:223 Hcxestrol ind phonoboi'Mtol, ^:201 Key word cards, 1:37, 1:108, 1.1167, 1:239, li335 HlllJn* F* t.fth Tlrthcs, S. liolak, W,, vit*A>in I*j ^ by atomic abfiorptlon, 6^:23 Hopas, X. >(., N,N-dU-Llivl lynergAinlde (LSD) and ISD-llke com Klrchhocfer, R. D., determination of decomposition product of diatepoa (valium eubatanee) by combined iostrumaotel tnelyala, 5.:16L pounds. 1. ftritkground information, 4:3 idontlflcation of >>SD by 1R spacerophotooetry, 4:26 multiple lntsrnel reflection spectroscopy, 4^211 Sag also Dow, M. L. 5e^e also Pullman, r,. W, Howard, 3. F., Teflon washers as heat shields for GLC Injection dlaphrcpma, J:36 liordlc, C., y/u: WntUngton, 7', M. Huron milk am) tissue, ppitlcldes In, by GLC, ^:205 ' Il'imUoy, J, G., ex&mlnotlon of sorbitol as its ttloathylsilyl ether by GLC, 3:169 Hutson, S. D., wnnlyala of the trlbutyrin (glyceryl tributyrate) content of butter as index of vegetable fat adulteration, 6:19 Hydrocortisone, effect on pyrogens tout for noomycin-hydrocorti- fonr tdjxttsn*, ):709 fbrnh/o, W,, new technique for preparation of TLC pistes, .1*333 IndoK, Bureau Ry-Llrea, Volumes 1-5, 1^:67 " Index, lnterburcau By-Lines, Volume l7 1:339 Volume 2, 2:302 ~ Volume 3, Vc lume 4, Z1311 Volume 5, 5:269 Infomatlon retrieval, column trap ehrotnstogrephy abstract#, 3:57 drug analyalw, 3:5, 5^:207 ~ koy word cardn, 1:37 Kitshbeum, A., automation of microbiological assays: yesterday, today, end tomorrow, 6:31 results of 2-yeir testing program of antiblotlea for con tamination by penicillin, 4_t49 Kletntnen, A., modify th method!, 2l187, 3.:306 Kllng, M. S., and Wells, C. GLC separstlon of optical isomer* of some eympethoslaetic amines, 4^:275 Knoll, E. W,, sea Bowmen, F. W. Koch, S. A., end Alexander, t. G., Investigations of spectral quality and minimum aampls ales on the A-60 NMX spectrometer, ^:49 Korte, D. E., sxtractablea in rubber materials used In food processing, 2,i63 Area, X. C., and Turctan, J. V., applications of NHR spectro- .scopy to regulatory drug analysis. 1. rapid assay of aelectad compound* by internal standard procedures, 6:257 Kras, T. C., Bellman, S. V., end Turctan, J. W., characterl- tatlon and determination of impurity found in dlstlllsd- - In-glaes acetonitrile by NHR and mats spectrometry, :233 Krebiozen case, scientific sspecte, 2.i245 ** Kriegsr, F. L., see. Taylor, J. T. pesticides, 3:35 DSW 033501 STLCOPCB4017463 Krlnlt.z, fii, eutomatoil data piocuaalng In Kloaiivoru piocurewit and Inventory control, 5:3J OfuUy to determine !touio>;*ncJtv of Insect fflth In Individual cartons of.Hr. .i5-* KflnHr, i>, t *;itl Fo.nno, A., Jr , .MjtoTi.u h1 d.ito prucc.'Jliiy, <h publication |>vocMre:':nC JI, ^:21.* LPJ, haj Luclnogen, atruefure elucidation, !:11) (corr. 5.: 170) Luk-ita, C. D., set- Vn/tioy, V. )\ Lnrl<`ic, J, p., jiiiov, K. B,, uuJ Simpson, R. F.t differentiation ol JiiV.a on 2 similar types of drug cnpnule* Ly noutron activation analysis, :95 l.aR,r.i!ui t iov hood*, f.r bJcrlHiy testing, JJMIO, C*190 I. anv, !>., and Salvln, M., oirotenold pi>-.nnin in Bhrlmp, 2^1*9 J, t vl, in f, ?.\?J in ^r-iln, rolnrof/vpc.y, 7:213 J.c. <i l 1 'Ulmony, liici.i'm < x ''qR, 1:59 (corr, .1:146) 11 i.t U !ev!dcmo, 3:JC'3, 3:Jvu I.jr , M, S., eye..1. i- bibliography, 6:43, 6199 r, M. , Dollmpio, D,, Green, S., Perry, H. , Harp, A., 0;vuld, E, J,, Lo:m, V., Solymosl, I,, and V.'ragg, J., rn\\ biology genetics and the FDA, 2:253 l.i'H'.i*.c, I!, \. , er)y pK-l'li r of the F1*A, 1:HI7 l.ct'.r to lift editor, 3 s 3<S iiv, identification of metical buttono (peyote), 4_t29 l1. A., rceiuorlul, 3:23f S'.*o .'lvo Jours, S, W.; l-uror, K, l.ljMcmb, c;, q. , chtc.U-nl opposition of Concotd grape Juice, 2:137 (corr, .3:94) l.oukdetermination of LSD and ieo-LSD by paper chromator p.:'ipby, : 19 field tftfct for LSD, 3:177 J. ow:ll, C., deterraln.'itVon of chlorpheniramine or dexfrroophen- iranine and phenylpropanolamine or lsoephodrina itt cold pwpHMtione, 3:81 LSD, ruo Lysergic arid d I nhylnuiideB UHtfg,"E., NMR literature retrieval by computer, 4:269 Lysergic ncid dlethyLamide, 2.5149, j2?l53, ^*31, ^*119 background Information, :3, 4:10, tl5, :16 Hold teat, 3:177 id aoroinx glory seeds, 1:97 1R, ):2S5, 4:24, 4:26 " paper chromatography, 4,:19 TLC, 4:21 d-l.yUTRlt acid dUthyUmtdo tartrate, fleh bloaeaay, 3.1201 Mackerel, Pacific or Jack species, Identification, 5:53 McCulloch, R, W., assay of amphetamine In formulations with thyroid, phenobarbitnl, atopina, and wloin, 4,:279 HeCowun, R. J., eniarion spectroscopy ana its application, i289 MeNuvnny, C P, Alternative method for vtauonity Bcaaurerent, 1:313 MeNer'ncy, F. C., and Boaver, L. A., datormlnatlon of tract amounts of trlchlorobcnxene In fooda, 5:195 Kaenaaium oxida, affact on nitroglycerin decoctpoaltlon, 4:193 Major, A., Jr.( and Crawford, R. H., daternlnatlon of liexachlorophena and reaorclool In praeanca of parabena, 1:105 Major, A., Jr., and Hall, M. J., determination of tin and iron In fruit drinks, 1:147 Kanske, D. D., and I rtBch, D. L,, ldantlf Icatlon of paatlddea by extraction g-valuca, 2^^^ ' Margnrlnoa, fatty acid concent, 2-.i Harino, V, 8., porous glaas aw TLC adsorbent, :6l Markovlia, A. 1., Improved ootUlty taat procodura, 5:241 Martin, H. P., kay word cards for slapla retrieval tyatea, 1:37, H10B X,Martin, R. see Riegnund, E. C, Martin, R. J., Dethcrt, D. D.,and Bayer, B., H,N-dlethyl lysoegaadie (LSD) and LSD^llka coapounda. II, analytical background, tl0 Haas epectronatryT dlaeapan dacoepoaition product, 5:161 N,H-dlethyl tryptanioa and ita intermediates, 5:27 iopurity In acatonitrlle, 6:2)3 practical applications, 1:28? Haas spectronetry-gaa chromatography, 6:192 MPA, f>)t o-siathyl*3,4-ethylana-dioxyphenethylejin Hoal, special differant 1st Ion by disc aloctrophoraais, 2^: 131 Mcclleine HC1, in drugs with pvrldt.xJnu MCI, 3:IS1 Meeth, E. , ami Foach, fi. L. , of t-'Nim rli lorfn.itvd peatirrj.j j,y t;.c, 2;?95 ' Melchior, l>, ( rr.ai:t i tutlvc <.-LC ,f xylenu ntul tfluotw in cctt'Un \.\U\i (riliinora and M.;:--*, 2:1-/. Mr n-sdl one uodHvi bisulfite, spre t r a:-*,.* i nmc! ry S: 2 3 5 Mcl'ils. fluoiid,:a in U / specific tluoride lectroi-c, 6:2o3 trace i y^i, M-rjy spectroscopy of totftl <Jlrt sunpica 4:1^5 ' Methenoaine, cl.t , 2:109 -Methyl -3,4-irci.hyloncdioxyphcncthy 1 amine, Idontificatlon, 4:271 Microbial enn lamination, blbl lography , 6:229, 6^:320 Microbiological utiflAya, automation of, 6:31 Microscopic method, for manure in dofry product*, 1:77 Miles, B. C., correlation of oreanoleptic evldcnco*'vith pH, votndle bases, and indole ns indices of decomposition In raw, frozen shrimp, 6:304 distinguishing between oxtriphylline and theophylline by TLC, 2:159 Hiller, C. A,, and Werren, J., frozen king crabocat drained walght study, 3:259 Hiller, L. C., letter to the editor, 3:306 Milk, chlorinated cioancer rufcidues In, 2:31 human, pesticides in, GLC, ^:205 Hinoral oil (white), In bakery products, 2^:297 on hard enudy, 3:47 Mitchell, L. C. celciua sulfate as an adsorbent for TLC, 3:?37 preparation of chroaatogrophlc piste for TLC: channel technique, 2^: 77 Kojd count and rot, in comminuted fruit, 1:213 Moisture, In comminuted vegetable spices, ,1:267 lose, cottage cheese cartons, Monochlorobenzene, contaminant In chloral hydrate, 1:297 Moor, J. L., Authentic data on prune julca eoncantrata and dried prune composition, 4.: 141 Hoqula, R. J., rapid identification of sugar* and sugar alcohols by paper chrooatography, 2^73 Morris, W., lead In total di'it sample# and typical fooda, 2:27 Morrison, J, C., and VerfellUe, J. R., apactrofluoromotrlc and TLC determination of quinldlna sulfata cootaminaclon In various drugs, 6:237 Motility, Improved test procidura, 5:241 House-skin painting study for carcinogenicity of 2 colors, :105 Mouthwash, bacterial growth In, 6:169 Kullar, H. J., genetic effect* of chemicals, 1:133 Multiple internal reflectance spectroscopy, ,4:211 Mutagenesis, chemical, 1:133 ~, Myeotoxlns, aflotoxln decontamination, 1:243 bibliography, 3:95, 3:134, 3:193, 3:2Tl, 4il33, 4:203, 4:237, 4:297, 5792, 5:133, 5:177, 5:120, 5:271, 6:54 - -- - lEdVz, 3:250 solvent contamination, 2^39 Myrick, J. W,, automation at National Canter for Drug Analysia, 5:37 Marrln, M. B., poetsT corner, 1:234 Heovycln In mixture with hydrocortisone, affact of hydro cortisone on pyrogen cast, .1:209 Neutron activation analysis, food products, bibliography, 6^:294 Ink on drug cepaulee, 4^:95 Mevton, J. M., analysis of undeeylenlc scld and Its salts In antifungal preparations by IR spectroscopy and polerography, 5:279 Niacin, with oiacioamide, 1^:91 Niacinamide, polarography, in multivitamins, 1:235 with niacin, 1:91 Nicotinamide, sea Nlaclnaalda Hlelso,.J. K,, and Goldstein, B, P., effect of hydrocortisone on the east for pyrogens In s neomycin-hydrocortisone suspension, .1:209 Nitrofureeone, in feed, l.tl51 Nitroglycerin, decomposition, with magnesium oxide, 4^:293 DSW 033502 STLCOPCB4017464  i..;,v .1 1 - pelfi, roi>lucil ;i:iu11 fciiJ.l, 4:2B5 r t .. . m\v\i .*. i . s.c.-ir',!, 3:23 . . ,-i ).r. J. r tic rv<-h.:i or, act loni trite iwpuricv, 6:233 .rofivajc hvjrocurbune, <ikyi and arvl halides, and alcohols, i : 1 17 diazepam decompoel Mon product, 161 liter..lure retrieval, 4:269 regulatory drug imulyein, 6257 spuctrol quality ar.d utn!r.:um anmple sire, .3:49 11 ictl'.v 1 cup-tetraniitr and t etrae thylituc- j'rnt amine, _3:163 turpvat 1 nec, 4: rt9 O'D-n.Ki, J. , Jr., -v V.'.is Valin, C. C. p(h, Vi??uihble, roarJtM-, n.afvurineft, fatly acid content, 2^5 OlcotrnrgarLnc, packaged, shrinkage, .3;287 Organoleptic analysis, ducoioposition odora in fish, :121 incubator eggs, JM59 ahrJ-.p* correlation vita chemical indices, m 304 Oswald, F.. J., see Lvp,.ttor( M. Oxalic acid, colorlavtrlc analysis, 3:85 Oxloy, II. H., microbial contuminotion bibliography, 6^52291 o;320 Oxtriphylline, differentiation from theophylline by TLC, 2:159 p-V'aluca pesticide analysis, 2;17i Page, 0. r.t qualitative and quantitative analysis of some barbiturates by GLC, 1:203 Paper chromatography, chlorinated pesticides, 3.:224 L5D and iso-LSD, 6tl9 auger and cugsr oleohols, 2^:73 Partbcns, effect on assay for hexachlorophenc and resorcinol, 1.: 105 Penicillin, contamination of antibiotics, 4:49 procaine, effect on sulfaffethatini analysis, 1:97 (corr. .2:90) Perry, H,, see Legator, H, " Ptlttcldu snoiysls, automatic GLC injection system, 6:57 extraction ^-values, ^2:171 human milk and tissue, 2:205 improved CLC column, 2:71 Interference by chlorinated cleansers, 2:31 values for TLC, 2*29$ radiological mossuroment of cholinesterase activity, :85 Pesticides, aldrin and dleldrin in sugar beots, ^21217 3:91 Banol, biochemical measurements of toxicity to rats,'2*177 chemical literature, 2*35 ' chlorinated, low moisture graini, 3:27 paper chromatography, 1:224 TLC, .1:85 ~ DDT, effects on central nervous system, 6:313 dlthloearbaastee, 1.7255, 2:177 " andrin and dleldrin on carrots, 1:263 organophosphates, review of chemistry, 2:103 polychlorinated biphenyls, affects on central nervous system, 1313 rodenticldas in bait samples, 4.:51 trlchlorobantene in foods, .5(195 Petroleum dlatillatee, identification by CLC, 6:9 Peyote (unseal buttons), identification, 4:29 Phenobsrbitsl, and hexestrol, .1:201 Phenols In drug combinations, by CLC, 2:21 Phenylephrine hydrochloride, in opthalmlc preparations, physio logical affects, :113 Phtnylmercurlc acetate, In drugs, by polarography, 2.i271 Phenylpropanolamine, in combination with other cold prepara tions, 3:61 Pleehocki, J. T., dye extraction methods la pharmaceutical analysis, 5:15 Post's Corner, 1:234 Polarlmotry, optical rotary dispersion, 5:81 Antifungal preparations, 5:279 Polarojjrapby, cad;nl<cn In f *. 1 u f f s f 4:107 chloroform linlnu.nl, j!s 161 diethylHtiibeatrol In animal f><d*, 1:307 gold :<-,dlun chiosruliaiv Inject jhlo*, _4:103 In dm,; 1>, J^:l iodlrio lr, vflmln:>, 2:229 (corr. 2:270) load In grain, 2:213 nltrr.rv:, with dt-ritee, 6:??9 phenyliicrcuric ici-idte in drug**, 2.:271 riboflavin, thiamine HC1, and niacinamide, 2S27L thallium in povderod malt extract, 2;H Polito, M. V., ami Cvleutc, />. C., poiarograpltic determination of thallium in powdered ciaLt extract, _2:11. Poll to, M. V,, and Romano, A., dr., dlfferentintIon and iden- 1:91Uflcotion of niacin and niacinamide in pharmaceuticals, Polychlorinated biphenyls, effects on central nervout. svetem, 6:313 * Polyethylene, contaminant in paper chromatography of chlorinated pesticides, 1:224 Ponder, C., drug stability and chemical Incompatibility, .5:23 Potter, V. C., see Stanley, E. R. Potter, W. C., and Stanley, E. R., interference of sodium p- aminobenzoate in analysis of sulfamethazine in medicated feeds, 2:91 Preservatives, sorbic acid in cheese, 2.:81 Prochatka, M., Csjan, R. J., and Fernandet-Flores, E., deter mination of dlethylstllbcetrol in animal feuds by oticlllographlc polarography, 1^:307 . Progesterone, with estrone end testosterone, 4:35 Propellents, in cosmetics, 1_: 219 Prunes and prune juice, authentic data, 183 4:141 Pseudomonas aeruginosa. In non-sterlle antibiotic produets, 5:157 . . Psilocybin, identification and quantitation, .3:107 Publications, automated procurement, 5(215 Publications list, 4:181 (corr. 4:222), 4:264, 4:308, 5:49, 5:101, 5:145, 5:187, 5:237, 5:288, 6:52, 6:108, 6:166, 6:219, 6:276, 6:320 " -- - Pyridoxins hydrochlotidj in drugs with meclltine hydro chloride, 2-183 Pyrogens, offset of hydrocortisone on test of neomycinhydrocortisone mixture, U209 Pyropiiosphste, In canned tuna fish, litl Quantity of contents compendiura: chease, packaged, shrinkage, i:9 (corr. 1:146), 1:15, 1:26, U91, 2:96, 2:98, 2: 100 crackers, filled, shrinkage in 2^:227 oleomargarine, shrlnkago, 2:^87 tea, shrinkage, .3:291 Quaternary aimoolum compounds, in foods, bibliography, 6:263 Qulnscrine hydrochloride, fluoromatry, 4^:255 Qulrtidine sulfate, contamination in drugs, 6_:237 Rader, B. R., determination of moisture In comminuted vegetable spices, .1:267 lUdloactlvity, measurement of cholinesterase activity, 4:85 Ratay, A. F., soe Ctuenfold, H. Ramoaker, D. L., see Reeves, H. P. Rauwolfla setnentina, by fluorometty, 6:288 Reeves, M. P., Hall, J. R., Yates, P. J., end Raumaker, D. L., comparison of 2 methods used in preparing frozen vegetables for bacteriological study, 4:189 Riboflavin, by poUrography, 3:271 Roach, C. L., see Hceth, C. Roberts, J. 1., colorimetric determination of formaldehyde in foods, .5*283 Roberts, L. A., fluorometrlc determination of sterols as choloeterol In egg noodles, 4:229 quantitative fluorometTic method for aalnecrlne and Its salts In drug preparation, *85 rapid fluorometrlc determination of quloecrine hydrochloride in drug preparations, 4:255 DSW 033503 STLCOPCB4017465 Korienticldcft in boito, screening, 4:51 Rodrick*, J, V., Cv-'hmnc* H. uui SioW.if, olv:ni con tamination frcr. vojnrlln ccr.'.-'ri.mta of fiberglass plove box, 3j?39 Rod: if.ucaA. J.* nonaqiirous tllrniiou of acids and banco In (fiiorpaccntlcftl enalysi*i 5:12j KcpnvJte, h., drug nomenclature, 3;307 infoTfwjtlonnl old* for druc, nrvilyatH, 3:5 Koini.no, A., Jr., reothod of analysis for L*D, 2:153 Set; alho Kriottz, B., Politn, H. V.f Turcznct, J. W. ft.'Sfr.tf tol n, J., F*ln, A., Rianchf, R., and Will lama, J., analysis of pyridoxin* hydioehlorid* and meclizine hydrochloride combined in tablets and elixir, _3?^J PcuorrJnol, with parnbens, jh 105 !`>S3, V., Lo,tutor, M. ib>t, in coc-tir.ui t:d fruit, 1_:213 RubbprttJoteii.il! used In food processing, extractives, 2:63 Salicylic a^id, o<i>arutlon fron, benzoic acid In Whitfield's ointment, 2:155 Salmonella, In frog logs, :69 Calvin, H,, ice J.airy, D. Baiumul, 0. r7, Brannon, W, L, und Hayden, A. L., IP. sp.ctrA of soma compound* of pharmaceutical interest, 1^3 Sanitation, of confectionary manufacturing, 5ti89 Schcriel, H., cathode ray polarography of tiboflavin, thiamine hydrochJovidt*, and niacinamide, 3:271 Schneider, J. E. , comparison of low temperature asher with vat ashing technique, :79 Scroggins, H. S., determination of carbaraone In feeds by colorimetric spectrophotometry, _2:237 Sellar, C., sen Blakely, J, Shapiro, R. C., wycotoxin bibliography,3:95, 3:134, 3:193, 3.241, *.! 133, *.203, 4:237. 4:297, 5:92, 5:135, 5:179, 5.1220, 5:271, ?:3i ~ __ _ Shell, In chocolat coproducts, :3? Shsrken, 8, polorographic method to identify and analyte chloroform in chloroform liniment, ,2:161 X-ray method of analysis, 6,1140 Sherken, 8., and Williams, J* C., deterninstioa of fluorides in solder fluxes using specific fluoride electrode, 6:225 Shrimp, carotenoid pigments, 2^:189 " decomposition, correlation of organoleptic a,id chemical teats, 6:304 Shrinkage, packaged cheese and cheese products, 1:9 (corr. 1*146), l.i 15, It26 packaged collage abates, ,2:95, ii96, 2:93, 2*100 packaged filled crackers,""2:227~ ~ packaged oloo^nrgsrina, 3:787 packaged tea, 2*291 Siegmund, E. C. ."'and Martin, R, J,, Identification and quantitative detarnlnetion of psilocybin in tablets, 3:107 Simon, H. possible mydriatic effect of collyrlua containing 0.152 phenylephrine hydrochloride In human and rabbit yes, tU3 Simpson, R. E, see Lambert, J, P, Smith, D. ., computer-assisted analysis, 5:73 Bnow, R. sop Limbert, J, P. *" Snow, S W., sea Andres, C* N. . Sobotka, T. J., differential affects of DDT and polychlorinated biphenyls on central nervous system, 6:313 Sodium *a&lnoboncoate,* interference In assay of fulfamathatlne in medicated feeds, 2l$l Solvent contamination, from fiberglass glove box, 3:239 Solvents, by combined CLC-oaaa spectrometry, 6:182 kerosene, in vood stein, 3:223 separation by CIC, :17S ~ turpentine, ,Ji283 "" xylene and toluene by CLC, 2*195, *219 Solyaosl, I., seo Legator, M* Sorbic acid, in cheese, 2:81 Sorbitol, CLC, 31169 ~ Spectra coapilaTion, Infrared, of drug*, 1:3 UV, of color addltlvea, 6:192 " 333 Spi'Ct rv.rh^r or*Mt ^*r . f.'K- 2A, Hirnculefea, .1_: 2 78 Speci topholor.cirlc irM;:, cleaning, l: M Sperlitv, A. K. , drr:i\r.po3sition of ultroy.lyrrrin in presence i/ 7 : 1 ^ 3 Spices, vegetable, m.ij..turo in, 1:267 SI.vjIHlv of dnj.'s, Slrfkclam, r;. S.. and ;-;!<!>on, B. R. , Si'i' triMon j-.mJ vpv.ctronhotcn-otric deturml nation <>f hf::cfltr\jl anJ phenobaibltel in tablet prcparetlonB, 1:701 Stanley, E. H., tec Potter. W. G. " Stanley, E. R., and hottt r, W. C., dctpni.inatic7n of sulfn*;rth,t- clne in medicated feeds containing procninn ponletlftn, 2:97 (corr. 2,9<>> Staphylococcus, enterotoxine In food, gcl-d!fluxion detection, 5:247 Statistical unslyslq, sample size foruiula, ?:15 (corr. 2:19) Statistical concepts in drug analysis. 6:J'/ " Stau.rlvr, L. J., updnclnr, analytical constants for gg content of food, 3:33 Stelnbrecher, It., collaborative study of deterMnotion of airjvonia aa Index of decoapoaltlon in crabneat, 6:281 Stephens, R. L., manuto In dairy products, 1:77 Sterility of antibiotics, 5:157 " Sterility testing, antibiotics, 3:1 lonlnar sir flow hoodnf 6:90 Steroids, abstracted bibliography, 6:161 estrone, progesterone, and testosterone, 4:35 GLC, 1:269 ** in antibiotic preparations, lntarferancee In assay, 2*279 natural estrogens, 3:225 Sterols, in egg products, 3:33, 4:229 Stoloff, L,, wee Rodrickw, J, V. Stoloff, L*, snd Trager, W., recommended decontamination procedures for aflatoxin, 1*243 Sucatyl, in dietary candy and chewing gum, 3:23 Sugars, in natural products, by GLC, 4:147 ~ monossccharidea by l'LC, 2*149 * sugar alcohols by paper chromatography, 2:73 Sulfamethazine in feeds, v: th procaine penicillin, _L:97 (corr. 2j90) interference of sodium p*eolnobensoate, 2:91 Sulfisoxarole end acetyliu?fisoxarole, Braiton-Harshall assay, 2;127 Sutor, R., end Libby, D. A., colorimetric determination of oxalic acid, 3:85 Sympathomimetics, GLC of optical isomers, 4:275 TLC, 4:261 ~ Szymanskl, H. A., see Barcklow, P. C. Xablet pulverisers, evaluation, 4^:197 Talley, M. C., FDA scientists occupy nev laboratory headquarters, 2:147 Tanner, J. T., and Frlsdaan, H., application of neutron activation analysis to food produets: bibliography, 6:294 Taylor, J. T., analysis of 3 drugs containing carblnoxaalne by GLC, 2:117 Taylor, J. T,, and Krlegar, E, L., rapid GLC analysis of methenaodne in pharmaceuticals, 2^: 109 Tea, PDA responsibilities under Tea AFt, l.:317 packaged, shrinkage study, Testosterone, with estrone and progesterone, 4:35 Thallium, polerography, In powdered melt extract, 2:11 Theophylline, differentiation from oxtriphylline b7 TLC, 2:139 Theper, H. E, determination of iron In drugs, ,2:241 Therapeutic equivalency, of drugs, 5:11 Thiamine HCl,.polarogTaphy, 3:271 Thin layer chromatography, calcium sulfate adsorbent, 3:237 channel technique, ,2:7? chlorinated pcatlclFea, l_t85 corticosteroids, 5:7 extraction apparatus, 2^:145 OSW 033504 STLCOPCB4017466 3 V, Hi 1 n layer cUri-mar c'nrarlr- (rent glroxln in d'.vlto^iu and dlroxtn tablets, 6:25 |,;D and LSD urfi-Hte, i:21 - 1 .*/.; H \ i :*: * t : 1/7 rW- IV,,: -.jri.Jo*, . r.;l'.9 c.xrri(>iivlU.v* ami thuoj.hvHlne, 2;>59 I'l ............... !: ' ) ,v'' oOs.*rKi-nt, 2,;6l ouin'dln* sulfate as contaminant In drugs, 6:237 Kp^> value* for chlorinated pesticides, 2:295 urine cor.: n*.l ,;.it lor., 2:2i3 tvporotion and id**nt i llection of autlHletealnes, _51171 h)'npthcniifretieb 4:i!bl triethyU-ne-ietraraino and tetraethyl one *pentamln#, 3:163 IhreiJur, J. Jr, .j^srrjct of literature on column ''trap0 <*.!". rciu.ilrr, t af-hy, 3: V 7 dele ruination t-f (ascot fragments nnd rodent hairs In whitn flour baked i.oodh ar.d alimentary paste* by modified acid hydrolynja method, 3:313 Thyroid assay, recent progress, ,3:125 Tin, in iruit drinks, \J\U7 1! 1 -,:. t>-n, no*i :juo-us teid.niquou, In dru analysis, 5:125 Ti'luvMi" In pairtl Uilnnrrs by CLC, .2:195 (corr. t}22j, jlJ2A9 Total diet analysis, arsenic, 1:251 ltjsd, 2:27 " troco analysis by X-ray spectroscopy, :165 Tr^por, V., see Siol.ofC, l. Txlbutyrln (glyceryl tributyrate), in butter, from vegetable fat contamination, 6:19 TrIchlorobcntant, CLC, (race amount* in foods, _5:195 Trlcicthylamino, In fifth decomposition, 2,:153 Torciatt, J, W., sun Bellman, S. V.; Kras:, T. C. Turcton, J. W., and Romano, A., Jr., separation and determina tion of salicylic and benzole acids in Whitfield's ointment, :1SS Turpentine, 2*263, V.B9 . Ur.bcr^or, t. J., therapeutic equivalency of drugs factors that can Influence biologic availability, 5:11 Undocylcnlc acid, In antifungal preparations, 5:279 Van Valin, C, C., Kalluan, B. J.t and Q'Doniiol, J. J., Jr>, polyethylene aft source of artifacts In paper chromato graphy of chlorinated hydrocarbon Insecticides, 2J**4 Vegetables, frotan, prepsrarlou for bacteriological studies, 4:189 Verfallllo, J. R., tee Horrlaon, J. C. Vlscoalty, alcernatlva to Saybolt Viscometer, Jh313 Vitamins, Sj2 by tonic abeorptic*, 6:23 D, Improving USP method, .2:) , iodine in, 2:229 (corr. 2*270) Benadlooe sodium bisulfite, 5:285 Olecin and niacinamide, 2*^1 niacinamide, 2**35 riboflavin, thiamine 8C1, and niacinamide, 3:271 WaeHngton, ?. H., Nordic, C.f and Heino, K. V., Jr., trace analysis of total diet samples by X-ray fluorescence spectroscopy, 6:165 Wayland, L. G., ear firecey, A. Webor, A. L., determination of pyrophosphate In canned tuna fish, 3:67 problem* in identificstlon of fiah apecles, snapper, 5:153 soma considerations in laboratory examination, detection, and interpretation of decomposition odor* in fish, 5:121 Weeks, J, F., Jr., Baird Model Ky-1 flame photometer: adaptation, adjustment, and calibration for general use, 2:163 guidelines for determination of conjugated estrogens, 4:)45 phenylpropanolamine hydrochloride, phenlranlne malaate, and pyrllamlnc aaLeate In syrup* by eoluaa chromato graphy and UV spectrophotometry, 6:85 Volk, R. V., see Werrcn, J, C, Walk, K* W. and Werrsn, J, C, packaged creamed cottage cheese shrinkage study at Sealtest Division, Uatlonai Dairy Products Carp., Chambersburg, Fa., and Washington, D, C,, 2:98 wvi-r, y. j., aec Braccy, A. p Wi.-M.-s C. K., f.*o Kling, M. S. Verrri\v J. C.. necknt'u rhorj* nd rheeee products shrinkage "t>irlv nt Kraft Foods, Springfield, Hibiouri, 1:15 T`,-dto Co., Pi vr.nuth, Wisconsin, 2***8 qmn* : contents cc.;w-nditin: packaged lea shrinkage ut'.dy, Sop .-.Mo Miller, C. A.; Walk. R. W. Kcrrcn, J. C>, and Blutaqulst, V. H., packaged cheese ahrlttkep,e study nt Borden Foods Co,, Van West, Ohio, 1:9 (corr. l:U6) Wetron, J. C., and Wclk, B. W., packaged creamed cottage cheese shrinkage study si Capitol Milk Producers Coop., Inc., Frederick, Hd., and Washington, D. C., 2?lOQ Snfcvay 8tote, Inc., handover. Hd., 2i97 quantity of contents corrpondJua: packaged oleomargarine shrinkage study, 3:287 klieclec, H. a., dried tig ond fig putts industry: relation of growing and processing practices to insect end filth content of finlehc.d product, 2!*5 insect filth in domestic fin pastes, jt:223 ' White, M., further studios ur,ing laminar etr flow for sterfjlty testing of pha.meoeutl.cftl droa*. 6:90 Whitfield's ointioent, separation of bensoic and salicylic acids, 2:155 Whiting, M. C., ascorbic acid and the common cold: selected references with annotations, ^229 Whitley, V. P., arsenic In total diet eample, l'-2^ determination of ereenlc In swine liver tissues, 2<165 method for doterfflination of ecctyl-p-nltrophcnyl sulfanilamide and 3,5-dinltrobencaalde in madlcated feed preulxea, 2i2f>) ` . Whitley, V. P., Joe, F. f.., Jr,, and Laketa, C. D., residue analysis of 3,5-dlnltrobencamlde (3,5-DNBA) In poultry tissue, :75 Viltmowskl, C., colorimetric determination of sorbic acid in cheeses, 2:81 spectropholometrlc method for dliodohydroxyquln In drugs, 6:179 Vllderman, M., shrinkage study of packaged filled cracker*, 2:227 Wilkie, J. B., sea Jonei, $, W. Wllliaras, C. H., and Caittrllne, J. L., Jr., sosa biochemical meaeureaents during chronic feeding of tb aarbaaats iano. to rata, A:17? Williams, J. C., tee Roionstein, J.) Sharken, S. Williamson, W, T., ill, poiaTographic determination of trace amounte of lead In grains and grain product*, 2;213 Womack, M. S., fish apecles Identification by diac elactro- phoreals, 2^81 Identification of colors using rapid strip electrophoresis, UZ27 Woodson, A. L,t snalyafa of drug* subject to drug abuse control act, 3:113 snalyeie of estrone, progesterone, and testosterone in a suspension vlthout separation, 4:35 assay of gold Sodium thiosulfate Injectable* using conventional polsrography, 6:103 determination of 3-nltro-4-hydroxypbnyl*r*onlc acid in feeds, , 4:285 -- polarographlc dataralnation of nitrate* in aqueous madia con taining nitrites, 6.1299 polsrography In drug analysis, 5:1 use of operational amplifiers In the laboratory, 6:119 Wragg, J., aoc Legator, H. " X-ray analysis, 6:140 total diet aamplas, 4ii65 Xylene In paint thlnnere by CLC, 2*195, 3:219 (corr. 4:222) Yarnall, F. E., pllllatlca, or identification of manufacturing source of barbiturate and amphetamine drug#, 3;127 Yates, P. J., see Reeves, M. P. Xachariac, h., 1R idantificarion of LSD In capsules, liquids, auger tubas, and tablets, 3:255, :24 Zaabarg, B., and Dies, R., TLC of some monosaccharides, 3:149 > tv t 11 OSW 033505 STLCOPCB4017467