Fluensulfone ... - IR-4 Project

ppm butene sulfonic acid =
0. 0009 g/mL
x 8.0 mL x 1x
66 mL
6.0 mL x 10 g
0. 0079 0.
000 ppm
Percent Recovery =
= 88%
0.01ppm
x 0.896
Time Required for Analysis
PTRL West Project No. 1977W
Report 2 Page 24
= 0.0079
Time required per sample set, where a sample set consists of twelve (12) matrix samples,
8 standards and 1 reagent blank:
Extraction and Clean-up take approximately 8 hours for one analyst
LC-MS/MS analysis and data processing takes approximately 28 hours
TOTAL = approximately 14 hours for one analysis (2 calendar days)
RESULTS AND DISCUSSION
Method validation was successfully conducted for MCW-2 and its metabolites M-3625
(thiazole sulfonic acid, TSA) and M-3627 (butene sulfonic acid, BSA) in tomatoes,
peppers, cucumbers and melons. The validations were conducted at 0.01 ppm and 0.10
ppm. The method validation results are summarized in Tables I through IV for tomatoes,
pepper, cucumbers and melons, respectively. The supporting data is provided in
Appendix C. Due to the chemical nature of the analytes, MCW-2 has one quantitation ion
and two confirmation ions. Both M-3625 and M-3627 have one quantitation ion and one
confirmation ion. Representative calibrant chromatograms and calibration curves are
presented in Figures 1 through 28.
Method validation for MCW-2, M-3625 and M-3627 in tomatoes was conducted with
two controls, five (5) replicates at 0.01 ppm and 5 replicates at 0.10 ppm. The average
percent recovery for MCW-2 was 106% at 0.01 ppm and 98% at 0.10 ppm. The overall
average percent recovery of MCW-2 in tomatoes was 102% with a standard deviation of
13%. The average percent recovery of M-3625 was 83% at 0.01 ppm and 84% at 0.10
ppm. The overall average percent recovery of M-3625 in tomatoes was 84% with a
standard deviation of 9%. The average percent recovery of M-3627 was 95% at 0.01 ppm
and 97% at 0.10 ppm. The overall average percent recovery of M-3627 in tomatoes was