Fluensulfone ... - IR-4 Project
Fluensulfone ... - IR-4 Project
Fluensulfone ... - IR-4 Project
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Retention Time: Butene sulfonic acid (M-3627) was ~6.5 minutes<br />
Thiazole sulfonic acid (M-3625) was ~7.7 minutes<br />
PTRL West <strong>Project</strong> No. 1977W<br />
Report 2 Page 21<br />
Separation of the analytes was achieved by HPLC. The analytes were identified by the<br />
coincidence of their retention times with the reference standards and MS characteristics,<br />
and quantitated by integration of the peak areas.<br />
A typical injection sequence for MCW-2 in a method validation set as analyzed by LC-<br />
MS/MS was: solvent blank, 0.5 ng/mL calibrant, 0.75 ng/mL calibrant, 1.0 ng/mL<br />
calibrant, 2.5 ng/mL calibrant, 5.0 ng/mL calibrant, 10 ng/mL calibrant, 25 ng/mL<br />
calibrant, 50 ng/mL calibrant, solvent blank, 0.5 ng/mL calibrant, 0.75 ng/mL calibrant,<br />
reagent blank, control sample, control sample, 1.0 ng/mL calibrant, fortified control,<br />
fortified control, fortified control, 2.5 ng/mL calibrant, fortified control, fortified control,<br />
5.0 ng/mL calibrant, fortified control, fortified control, fortified control, 10 ng/mL<br />
calibrant, fortified control, fortified control, 25 ng/mL calibrant, 50 ng/mL calibrant, QC<br />
standard. The initial injection of calibrants was used to generate the calibration curve and<br />
the interspersed calibrants were used as quality control samples to insure the stability of<br />
the analysis throughout the sequence. A similar injection sequence was used for butene<br />
sulfonic acid and thiazole sulfonic acid analysis.<br />
Statistical Methods<br />
The residue data included the following statistical calculations: means, standard<br />
deviations, relative standard deviations and linear regression analysis.<br />
Limit of Quantitation<br />
The limit of quantitation was assigned as the lowest fortification level of analyte<br />
validated by the residue method. The LOQ for MCW-2, butene sulfonic acid sodium salt<br />
(M-3627) and thiazole sulfonic acid sodium salt (M-3625) in tomato, pepper, cucumber<br />
and melon was 0.01 ppm. The limit of detection was assigned as the lowest calibrant used<br />
in the analysis or 0.5 ng/mL MCW-2 and 0.45 ng/mL butene sulfonic acid and thiazole<br />
sulfonic acid.