Document 2jQeE0rGxKLDGYDa6D9rww43a
DuPont Haskell Laboratory for Health and Environmental Sciences
TO: FROM:
M R FPL!B
[POCKET H-24691
J. C. MASLANKA
TEST SUBSTANCE STABILITY OF
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August 5, 2002 cc: G. A. Ladies
Medical Research Project Number: Haskell Sample Number: Analytical Test Code: Analytical Report Number:
Notebook References:
Attached is the analytical report f'or tjhftstudv iidentified above. This analysis was performed to satisfy protocol requirements for " # 5 ut may also be used for other purposes.
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TEST SUBSTANCE STABILITY O
Medical Research Project Number: Haskell Sample Number: Analytical Report Number:
HA-2002-055
SUMMARY
A sample o f f l p H H H H H H H P H p a s received May 22,2002, and analyzed May 30, 2002.
The percentage o f active ingredient (a.i.) was measured to be 101.8% + 2.9 w it ^ r a n g e o f 99.5
to 105.0% for replicate analyses (n = 3). The sponsor reported a purity o l f lM B v h e n sample
was submitted.
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SIGNATURES:
A nalysis by:
Richard! F. Rossi Chemistry A ssociate
Report by:
Lvicb C-
' Janet C. Maslanka
Senior Staff Chemist .
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Date
r- 200
Date issued:
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HA-2002-055 page 2 of 3
METHODS
Analysis for the percentage of a.i. in a sample o: chromatography (GC). Sonication in methanol was requiredior internal standard and analytical standard stock to ensure that] completely dissolved.
as performed by gas aration of test substance,
as
SAMPLE PREPARATION & ANALYSIS
Aliquots (0.0399, 0.0334, 0.0384 grams)
dissolved in methanol
(100 mL) to give nominal concentrations of 399, 334, and 384 ppm. T he aliquots were further diluted
to a nominal concentration o f 23.9, 20.0,23.0 ppm, respectively, and analyzed according to the
following method.
INSTRUMENT & CONDITIONS
Instrument:
Hewlett-Packard Model 6890 GC
Column:
J&W DB-1701, 30 M, 0.32 mm ID, 1.0 pm film thickness
Injector:
Split, 250C
Detector:
FID; 250C
Carrier Gas:
Helium (2.1 mL/min)
Split vent:
45.1 mL/min
Injection Volume:
2 microliter
Oven Program:
Gradient
Initial Temperature: 100C
Initial Time:
1.0 min.
Level 1 Rate:
20C/min.
Level 1 Temperature: 260C
Level 1 Time:
0.00 min.
Total run time:
9.00 min.
CALIBRATION & QUANTITATION c. Calibration and Q uantitation
An analytical s t a n d a r d H H H H H ^ m m | ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ n v a s purchased from Fluorochem USA for the analysis. A stock solution w as prepared in1 methanol. This stock solution was sonicated to assure that all m aterial was in solution. Calibration solutions o f approximately 10.64 to 42.56 ppm were prepared in methanol. A sjppk solution o f internal standard! was prepared in methanol a m added to each calibratioifstandard and test solution to give a final concentration o f 40 ppm. The ratio o f the internal standard anc peak heights from replicate GC analysis o f these solutions w ere usectTo construct a calibration curve by least squares regression. M easured concentrations for each purity solution were determined by applying the peak height ratios from replicate injections o f each sample to the calibration curve.
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HA-2002-055 page 3 of 3
RESULTS
eluted from the GC column as reso, 'approximately 3.4 minuses. The sponsor reported a purity o: submitted.
with a retention time of rhen the sample was
Table 1. The percent of a.i. in the]
Aliquot 1 2 3
23.9 20.0 23.0
ample analyzed May 30, 2002
Percent Measured Nominal
25.1 105.0 19.9 99.5 23.2 100.9
Average Percent Nominal Standard Deviation Coefficient of Variation
101.8 2.9 3%
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