108139-1 Study Title Data Requirements Author Study ... - IR-4 Project

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Bayer Corporation <strong>108139</strong>-1 Agriculture Division 16. Shake the separatory funnel for 30 s. 17. Drain the lower organic phase into a 60-mL I-Chem vial through a funnel containing a glass wool plug and approximately 15 g of anhydrous sodium sulfate. 18. Wash the sodium sulfate with approximately 10 mL of methylene chloride. 19. Evaporate to dryness on a Turbo Vap LV (water bath 40 ± 5° C). 20. Reconstitute the residue in 25 mL of hexane. 21. Proceed to the Florisil clean-up (Sec 3.4.3.4, Step 1) 3.4.3.2 Extraction (Nutmeat) 1. Weigh 5.00 g (± 0.02 g) of the sample into a paper thimble for the soxtec. Begin recovery samples at this point by fortifying the control tissue matrix samples with a standard. 2. Add 50 mL of hexane to the soxtec stainless steel beaker. 3. Place the cup on the soxtec and extract ~ two hours at 140 °C in the boil position. 4. Turn the soxtec to the rinse position and rinse for 1 h. 5. Allow the cups to cool to room temperature. 6. Add the d6-cyfluthrin internal standard (0.05 ppm) to the soxtec cup. 7. Transfer the sample to a 50-mL graduated cylinder. 8. Wash the soxtec cup with 5 mL of clean hexane and transfer to the graduated cylinder. 9. Bring the volume in the graduated cylinder to 50 mL with hexane. 10. Proceed to the ACN / hexane partition (Sec 3.4.3.3, Step 1) 34
Bayer Corporation <strong>108139</strong>-1 Agriculture Division 3.4.3.3 ACN/Hexane Partition 1. Transfer 25 mL of the sample from the 50-mL graduated cylinder to a 125-mL separatory funnel. 2. Add 25 mL of ACN presaturated with hexane to the separatory funnel and shake for approximately 30 s. 3. Transfer the lower ACN layer to another 125-mL separatory funnel already containing 10 mL of hexane presaturated with ACN and shake for approximately 30 s. 4. Collect the lower ACN layer into a 60-mL I-Chem vial. 5. Repeat Steps 2 through 4. Note: Both ACN fractions in Step 13 are collected in the same 60 mL vial. 6. Concentrate the sample in the 60-mL vial to dryness on a Turbo-vap LV (water bath 45 ± 5 °C) and reconstitute in 25 mL of hexane followed by sonication. 7. Proceed to the Florisil Clean-up (Sec 3.4.3.4, Step 1) 3.4.3.4 Florisil Clean-up 1. Place a plug of glass wool at the bottom of a Kontes column (11 mm ID x 250 length, 200 mL reservoir), and add 50 mL of hexane to the column. 2. Slowly add approximately 7 g of 2.5% deactivated florisil into the column while tapping the column to remove air bubbles. 3. Add approximately 3 g of anhydrous sodium sulfate to the column. 4. Drain the hexane until it is just above the sodium sulfate layer. Discard the hexane. 5. Pour the 25-mL sample extract from Step 20 (extraction for all matrices except apple, pear, and nutmeat) or Step 6 (ACN / hexane partition nutmeat) into the column. Let the extract run through the column dropwise. Discard the hexane. 6. Wash the I-Chem vial with 40 mL of hexane and transfer to the column. Allow the hexane to drip until it just reaches the top of the sodium sulfate. Discard the hexane. 7. Elute the analyte with 40 mL of hexane/acetone (9:1) dropwise into a 60-mL I-Chem until no more drops are apparent. 35
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108139-1 Study Title Data Requirements Author Study ... - IR-4 Project

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