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

Bayer Corporation 108139-1
Agriculture Division
45 mL of MeOH into the bottle. Homogenize for 2 min, then filter a second time
into the same stoppered 100-mL graduated cylinder.
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solution to the filtrate. Adjust the volume to the 100-mL mark with the solvent
mixture and mix.
6. Split the 100-mL filtrate into two 50-mL portions and discard the filter.
7. Rotovap one of the 50-mL sample portions to remove all the solvents as possible
(some matrices may contain oily residues that can not be evaporated). Add
25 mL of hexane to the flask, sonicate in a water bath for 60 s.
8. Proceed to the florisil clean-up step.
3.4.2.2 Florisil Clean-up
1. Place glass wool at the bottom of a Kontes column (15 mm ID x 250 mm length,
250 mL reservoir), add 100 mL of hexane to the column.
2. Add 7 g of 2.5% deactivated florisil into the column and tap the column to remove
the air bubbles.
3. Add 6 g of anhydrous sodium sulfate to the column and drain the excess hexane
into a waste container. Leave enough hexane in the column just to cover the bed
of sodium sulfate.
4. Pour the 25-mL hexane sample extract from step 7 of the extraction into the
column. Let the extract run through the column dropwise into a waste container.
5. Add 40 mL of hexane to the boiling flask, mix and pour into the column. Let the
extract run through the column dropwise into a waste container.
6. Elute the analyte with 60 mL of hexane/acetone (90/10%) dropwise into a
125-mL boiling flask.
7. Rotovap to dryness.
3.4.2.3 Final Extract Preparation for Analysis
1. Pipet 2.5 mL of toluene into the flask and rotate to dissolve all the residue.
2. Filter approximately 1 mL of the sample solution into a sample vial using a
P -mm, acrodisc filter for GC/MS analysis.
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