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Fluensulfone ... - IR-4 Project

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PTRL West <strong>Project</strong> No. 1977W<br />

Report 2 Page 15<br />

acid sodium salt (M-3625) fortification solution was prepared by diluting 2 mL each of<br />

the respective 50 µg/mL working solutions to 10 mL in a 10 mL volumetric flask, where<br />

the solution was brought to the mark with acetonitrile:water (1:1). A 1.0 µg/mL mixed<br />

fortification solution was prepared by diluting 0.2 mL each of the respective 50 µg/mL<br />

working solutions to 10 mL in a 10 mL volumetric flask, where the solution was brought<br />

to the mark with acetonitrile:water (1:1). Due to suspected glassware carryover of the<br />

acid metabolites, reuse of these volumetric flasks was avoided.<br />

Sample Fortification<br />

Portions of control matrices (10 g) were fortified with MCW-2, butene sulfonic acid<br />

sodium salt (M-3627) and thiazole sulfonic acid sodium salt (M-3625) in replicates (5),<br />

as shown below, for determination of method recovery.<br />

Fortification Level<br />

(ppm)<br />

Volume of Mixed Fortification Solution<br />

0.01 0.10 mL of 1.0 µg/mL Mixed Fort. Soln.<br />

0.10 0.10 mL of 10 µg/mL Mixed Fort. Soln.<br />

Preparation of Calibrants<br />

All calibrant dilutions were prepared in amber bottles using appropriate pipettemen and<br />

disposable tips to dispense mixed standard solutions and solvents. An 5.0 µg/mL mixed<br />

stock standard solution was prepared by combining 1 mL each of the 50 µg/mL stock<br />

standards and diluting with 7 mL of acetonitrile:water (1:1, v/v) in a disposable amber<br />

glass bottle. The solution was sonicated prior to use. The following dilutions were<br />

prepared in disposable amber vials and diluted with acetonitrile:water (1:1, v/v).

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