Abu-Qare A W, Abou-Donia M B
Department of Pharmacology and Cancer Biology, Duke University Medical Center, Durham, North Carolina 27710, USA.
J Anal Toxicol. 2001 May-Jun;25(4):275-9. doi: 10.1093/jat/25.4.275.
A high-performance liquid chromatographic (HPLC) method was developed for the separation and quantitation of the insecticide chlorpyrifos (O,O-diethyl-O[3,5,6-trichloro-2-pyridinyl] phosphorothioate), its metabolites chlorpyrifos-oxon (O,O-diethyl-O[3,5,6-trichloro-2-pyridinyl] phosphate) and TCP (3,5,6-trichloro-2-pyridinol), the insecticide permethrin (3-(2,2-dichloro-ethenyl)-2,2-dimethylcyclopropanecarboxylic acid-(3-phenoxyphenyl) methylester), and two of its metabolites, m-phenoxybenzyl alcohol and m-phenoxybenzoic acid, in rat plasma and urine. The method is based on using C18 Sep-Pak cartridges for solid-phase extraction and reversed-phase HPLC. The compounds were separated using a gradient of 1 to 80% acetonitrile in water (pH 3.2) at a flow rate ranging between 1 and 1.5 mL/min in a period of 17 min and gradient UV detection ranging between 210 and 280 nm. The retention times ranged from 9.3 to 14.5 min. The limits of detection ranged between 20 and 150 ng/mL, whereas the limits of quantitation were 150-200 ng/mL. The respective average percentage recoveries of chlorpyrifos, chlorpyrifos-oxon, TCP, permethrin, m-phenoxybenzyl alcohol, and m-phenoxybenzoic were 78.6 +/- 6.4, 72.8 +/- 6.8, 84.8 +/- 8.0, 79.2 +/- 8.4, 80.5 +/- 7.2, and 82.3 +/- 7.1 from five spiked plasma samples and 77.5 +/- 8.1, 72.8 +/- 8.3, 79.9 +/- 6.4, 79.1 +/- 8.9, 80.5 +/- 7.6, and 81.4 +/- 7.8 from urine samples. The relationship between peak areas and concentration was linear for concentrations between 200 and 2,000 ng/mL. This method was used to analyze these chemicals and metabolites following dermal administration in rats.
建立了一种高效液相色谱（HPLC）方法，用于分离和定量大鼠血浆和尿液中的杀虫剂毒死蜱（O,O-二乙基-O-[3,5,6-三氯-2-吡啶基]硫代磷酸酯）、其代谢产物毒死蜱-氧磷（O,O-二乙基-O-[3,5,6-三氯-2-吡啶基]磷酸酯）和TCP（3,5,6-三氯-2-吡啶醇）、杀虫剂氯菊酯（3-(2,2-二氯乙烯基)-2,2-二甲基环丙烷羧酸-(3-苯氧基苯基)甲酯）及其两种代谢产物间苯氧基苄醇和间苯氧基苯甲酸。该方法基于使用C18 Sep-Pak柱进行固相萃取和反相HPLC。化合物在17分钟内以1至1.5 mL/分钟的流速，采用水（pH 3.2）中1%至80%乙腈的梯度进行分离，并在210至280 nm范围内进行梯度紫外检测。保留时间为9.3至14.5分钟。检测限在20至150 ng/mL之间，而定量限为150 - 200 ng/mL。从五个加标血浆样品中，毒死蜱、毒死蜱-氧磷、TCP、氯菊酯、间苯氧基苄醇和间苯氧基苯甲酸的各自平均回收率分别为78.6±6.4、72.8±6.8、84.8±8.0、79.2±8.4、80.5±7.2和82.3±7.1，从尿液样品中分别为77.5±8.1、72.8±8.3、79.9±6.4、79.1±8.9、80.5±7.6和81.4±7.8。在200至2000 ng/mL的浓度范围内，峰面积与浓度之间呈线性关系。该方法用于分析大鼠经皮给药后这些化学物质和代谢产物。
