高分子相間移動触媒を用いる水溶性薬毒物の抽出-誘導体化について(第1報)ジアルキルリン酸類のペンタフルオロベンジル化による高感度分析

The analyses of dialkylphosphates, aqueous metabolites or degradation products of organophosphorus pesticides, with extractive pentafluorobenzylation in the presence of polymeric phase-transfer catalysts (tri-phase catalysts) were investigated. Dialkylthiophosphates and dialkyldithiophosphates (alkyl=methyl, ethyl) in aqueous samples were extracted and derivatized in more than 98% yield by pentafluorobenzyl bromide in 15 min at 40°C using tri-n-butyl methyl phosphonium bromide polymer bound as a tri-phase catalyst and MIBK as an organic solvent. Dimethylphosphate and diethylphosphate were also derivatized in 43% and 100% yields, respectively, in the presence of this tri-phase catalyst in 90 min at 90°C. The simultaneous analyses of these 6 phosphates in the spiked urine sample were carried out with excellent detection limits, 0.44-0.79 ppm by scan-mode GC-MS and 0.027-0.081 ppm by ECD-GC) using this tri-phase procedure.