Method for the determination of captan metabolites in milk and bovine tissue samples by gas chromatography with mass-selective detection
1995
Kukla, D. | Wiebe, L.A. | Davy, G.S. | Atreya, N.C. | Clark, S.
A method for the simultaneous determination of residues of five possible metabolites of captan, 1,2,3,6-tetrahydrophthalimide (THPI), cis-3-hydroxy-1,2,3,6-tetrahydrophthalimide (C3), cis-5-hydroxy-1,2,3,6-tetrahrahydrophthalimide (C5), trans-3-hydroxy-1,2,3,6-tetrahrahydrophthalimide (T3), and trans-5-hydroxy-1,2,3,6-tetrahydrophthalimide (T5), has been developed. Tissue and milk samples are macerated with acetone and centrifuged. An aliquot of the extract is diluted with ethyl acetate, and the solution is dried over anhydrous sodium sulfate. The residuum obtained after evaporation of the solvent under a stream of dry nitrogen is partitioned between hexane and acetonitrile to remove lipids. After a silica column cleanup, the metabolites are derivatized by heating with N,O-bis(trimethylsilyl)trifluoroacetamide containing 10% trimethylchlorosilane. The trimethylsilyl derivatives are quantitated by gas chromatography with mass-selective detection. The mean recoveries and coefficients of variation (CV) from the analysis of 145 fortified milk, fat, kidney, liver, and muscle samples were as follows: THPI, 91.1% (CV 15); T3, 93.4% (CV 16); T5, 92.6% (CV 17); C3, 95.1% (CV 14); and C5, 88.5% (CV 19), respectively. The fortification levels ranged from 0.01 to 1.0 microgram/g.
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