Holstege D M, Scharberg D L, Tor E R, Hart L C, Galey F D
University of California, California Veterinary Diagnostic Laboratory System, Davis 95616.
J AOAC Int. 1994 Sep-Oct;77(5):1263-74.
A multiresidue screen for the quantitative determination of 43 organophosphorus, 17 organochlorine, and 11 N-methyl carbamate insecticides in 10 g of plant or animal tissues is described. The insecticides are extracted with 5% ethanol in ethyl acetate (v/v). Samples with high lipid content are cleaned up by automated gel permeation chromatography with a 30% ethyl acetate in hexane (v/v) eluant and in-line silica gel minicolumns. Highly pigmented samples are cleaned up with class-specific solid-phase extraction columns. The concentrated extracts are analyzed by selective detection with gas chromatography or liquid chromatography. Recovery of 71 insecticides ranged from 77 to 113%. Analysis of fortified bovine liver (n = 5) resulted in an average recovery of 96 +/- 4% at the 0.5 to 0.05 micrograms/g level. Analysis of fortified alfalfa hay (n = 5) resulted in a mean recovery of 94 +/- 4% at the 0.06 to 0.5 micrograms/g level, and analysis of fortified fresh tomatoes (n = 5) resulted in an average recovery of 97 +/- 3% at the 0.06 to 0.5 micrograms/g level. Method detection limits ranged from 0.02 to 0.5 micrograms/g for the compounds studied with a nominal 10 g sample.
本文描述了一种多残留检测方法，用于定量测定10克植物或动物组织中的43种有机磷、17种有机氯和11种N-甲基氨基甲酸酯类杀虫剂。杀虫剂用5%乙醇的乙酸乙酯溶液（v/v）提取。脂质含量高的样品通过自动凝胶渗透色谱法净化，洗脱液为30%乙酸乙酯的正己烷溶液（v/v），并使用在线硅胶微柱。色素含量高的样品用特定类别的固相萃取柱净化。浓缩提取物通过气相色谱或液相色谱选择性检测进行分析。71种杀虫剂的回收率在77%至113%之间。对添加了杀虫剂的牛肝（n = 5）进行分析，在0.5至0.05微克/克水平下，平均回收率为96±4%。对添加了杀虫剂的苜蓿干草（n = 5）进行分析，在0.06至0.5微克/克水平下，平均回收率为94±4%；对添加了杀虫剂的新鲜番茄（n = 5）进行分析，在0.06至0.5微克/克水平下，平均回收率为97±3%。对于标称10克的样品，所研究化合物的方法检测限为0.02至0.5微克/克。
