Document baqzJmg8KewBeQ2G3NgqaNpQZ

AR226-3267 449 DuPont Haskell Laboratory for Health and Environmental Sciences AR226-3267 March 6, 2003 cciMrI m I Qualify Assurance TO: FROM: MRFILi POCKET H-25425 J. C. Maslanka TEST SUBSTANCE STABILITY O F H-25425 Medical Research Project Number: Haskell Sample Number: Haskell Reference Standard Number: Analytical Test Code: Analytical Report Number: Notebook References: ^25425 Attached is the analytical report for the study identified above. This analysis was performed to satisfy protocol requirements for test substance stability but may also be used for other purposes. <**** i. TEST SUBSTANCE STABILITY OF H-25425 Medical Research Project Number: Haskell Sample Number: Analytical Report Number: HA-2003-032 A sample of H-25425 was submitted on February 26, 2003 a n ^ n a ly z e d g n February 27, JThyM rcentage o f active ingredient (a.i.) was measured to b e B H H H B i r i t h a M B f nominal for replicate analyses (n = 3). The sponsor reported a purity o; the sample was submitted. ACKOWLEGEMENTS Sample preparation by Sheila A. Riley (Chemistry Associate). Sample analysis by Bogdan Szostek (Senior Research Chemist). SIGNATURE Report by: Date Issued: <^L<^r Janet C. Maslanka Analytical Staff Chemist iff - H *<t>ts - b oO S - Z0 0 3 Date ^ TSCl HA -2003-032 page 2 of 2 METHODS Analysis for the percent of a.i. in a sample o f H-25425 was by high-performance liquid chromatography (HPLC) with a Gel Permeation Column (GPC) and refractive index detector according to the following method. Sonication was used to completely dissolve the test substance and the analytical standard stock solution. SAMPLE PREPARATION & ANALYSIS Aliquots (0.0403, 0.0417 and 0.0409 grams) of H-25425 were dissolved in tetrahydrofuran (10 mL) to give nominal concentrations of 4030, 4170, and 4090 ppm, respectively. CHROMATOGRAPHIC CONDITIONS Instrument: Column: Mobile Phase Flow Rate: Injection Volume: Column Temperature: Detection: Hewlett-Packard Model 1100 HPLC Styragel HR 4; 7.8 mm x 300 nom (GPC column) 100% tetrahydrofuran (THF) 1.0 mL/min 50 fil 35C Refractive Index CALIBRATION & QUANTITATION A separate sample of H-25425 test substance was designated as the analytical reference standard (93.17% pure). A stock solution of H-25425 in tetrahydrofuran was used to make calibration solutions that bracketed the test solutions. Peak heights from replicate HPLC/GPC/RI analysis of each calibration solution were used to construct a calibration curve by least-squares regression. Measured concentrations for each test solution were determined by applying respective peak heights to the calibration curve. RESULTS H-25425 eluted from the HPLC column as a resolved p>i ^k witjj^ rietention time o f about *l V9.023 0.02 minutes. The sponsor reported a purity olW t * hen the sample was submitted. Table I. The percent of a.I. in the H-25425 sample analyzed February 27,2003 . Aliquot ____ EE2LH-25425 Percent Nominal Measured Nominal 1 4030 2 4170 3 4090 Average %Nominal Standard Deviation Coefficient of Variation 3730 92.6 3790 90.9 3780 92.4 92.0 0 .9 1% CompanySaMNtasA notcontain TSCA CB1