Fluensulfone ... - IR-4 Project

3. Add 50 ml of ACN:HPLC water (1:1, v/v) to each bottle.
PTRL West Project No. 1977W
Report 2 Page 17
4. Tissuemize for approximately 5 minutes. Rinse probe with 10 mL of ACN:HPLC
water (1:1, v/v). Total volume 60 mL.
5. Place bottles onto wrist action shaker for 5 minutes
6. Transfer 30 mL of extract into 50 mL centrifuge plastic tube.
7. Centrifuge at 2,000 rpm for 10 minutes
8. Transfer aliquot of the supernatant to a snap-top GC vial for the direct MCW-2
analysis. Microfilterfuge the sample as needed.
9. Transfer 6.0 mL of the supernatant to 10 mL plastic centrifuge tube. Concentrate
sample to 3 mL in Turbo-vap at ~35ºC.
SPE Clean-up
10. Condition the Bond Elut 500mg, 6cc SPE cartridge with 5 mL of ACN, then 5 mL
of water.
11. Apply concentrated extract from step 9 and collect the eluate into a clean plastic
graduated tube.
12. Rinse the sample tube from Step 9 with 5 mL of water, apply to the same
cartridge and collect the eluate into the same graduated tube. Record the volume.
Total volume should be about 8 mL. Mix the sample by vortexing.
13. Aliquot in snap-top vials and analyze on LC-MS/MS for butene sulfonic acid and
thiazole sulfonic acid.
Note: In an effort to correct for the moisture derived from the matrix, three representative
samples from each matrix were extracted as described in steps 1 through 5 and the
samples were vacuum filtered through a Büchner funnel fitted with Whatman GF/A filter
paper. The resultant extract volumes were measured. The average volumes were 66 mL
for tomato, cucumber and green pepper and 63 mL for melon.