Di Muccio A, Pelosi P, Camoni I, Attard Barbini D, Dommarco R, Generali T, Ausili A
ISS-Istituto Superiore di Sanità (National Institute of Health), Rome, Italy.
J Chromatogr A. 1996 Nov 22;754(1-2):497-506. doi: 10.1016/s0021-9673(96)00535-3.
A rapid procedure has been developed that allows a single-step, selective extraction and cleanup of organophosphate (OP) pesticide residues from milk dispersed on solid-matrix diatomaceous material filled into disposable cartridges by means of light petroleum saturated with acetonitrile and ethanol. Recovery experiments were carried out on homogenized commercial milk (3.6% fat content) spiked with ethanolic solutions of 24 OP pesticides, viz., ethoprophos, diazinon, dimethoate, chlorpyrifos-methyl, parathion-methyl, chlorpyrifos-ethyl, malathion, isofenphos, quinalphos, ethion, pyrazophos, azinphosethyl, heptenophos, omethoate, fonofos, pirimiphos-methyl, fenitrothion, parathion, chlorfenvinphos, phenthoate, methidathion, triazophos, phosalone, azinphos-methyl, at levels ranging for the different OP pesticides from 0.02 mg/kg to 1.11 mg/kg. Average recoveries of four replicates were in the range 72-109% for the different OP pesticides, with relative standard deviations (R.S.D.) from ca. 1 to 19%, while dimethoate and omethoate were not recovered. Coextracted fatty material amounted to an average of about 4.0 mg/ml of milk. The extraction procedure requires about 30 min. The main advantages are that extraction and cleanup are carried out in a single step, emulsions do not occur, several samples can be run in parallel by a single operator, reusable glassware is not needed and simple operations are required.
已开发出一种快速方法，该方法可通过用乙腈和乙醇饱和的轻质石油，对填充在一次性柱中的固体基质硅藻土材料上分散的牛奶中的有机磷（OP）农药残留进行单步选择性萃取和净化。对添加了24种OP农药乙醇溶液的均质商业牛奶（脂肪含量3.6%）进行了回收率实验，这24种农药分别是：丙线磷、二嗪农、乐果、甲基毒死蜱、甲基对硫磷、乙基毒死蜱、马拉硫磷、异柳磷、喹硫磷、乙硫磷、吡唑硫磷、益棉磷、庚烯磷、氧乐果、地虫硫磷、甲基嘧啶磷、杀螟硫磷、对硫磷、氯芬磷、稻丰散、杀扑磷、三唑磷、伏杀硫磷、甲基谷硫磷，添加水平因不同OP农药而异，范围为0.02 mg/kg至1.11 mg/kg。不同OP农药四次重复的平均回收率在72 - 109%之间，相对标准偏差（R.S.D.）约为1%至19%，而乐果和氧乐果未被回收。共萃取的脂肪物质平均约为每毫升牛奶4.0毫克。萃取过程约需30分钟。主要优点是萃取和净化在一步中完成，不会形成乳液，单个操作人员可并行处理多个样品，无需使用可重复使用的玻璃器皿，且操作简单。
