论文标题:固相萃取—气相色谱法测定饮用水中15种农药残留
Multi-residue Determination Method of Pesticides in Drinking Water by Solid-phase Extraction Followed by Gas Chromatography with Electron Capture Detector
论文作者
论文导师 黎源倩,论文学位 硕士,论文专业 营养与食品卫生学
论文单位 四川大学,点击次数 121,论文页数 45页File Size2153K
2007-05-01论文网 http://www.lw23.com/lunwen_106493382/
solid-phase extraction ;; pesticide;; gas chromatography;; drinking water
目的：建立同时检测饮用水中15种农药残留的固相萃取-气相色谱分析方法，所检测的农药包括5种有机磷：敌敌畏，乐果，甲基对硫磷，马拉硫磷，对硫磷；5种有机氯：五氯硝基苯，狄氏剂，环氧七氯，α-硫丹，β-硫丹；5种拟除虫菊酯：甲氰菊酯，三氟氯氰菊酯，氯氰菊酯，氰戊菊酯，溴氰菊酯。方法：利用ENVI-C_(18)固相萃取小柱提取水样中农药，小柱用甲醇和水活化，丙酮-正己烷(25：75，v／v)洗脱，浓缩后用GC-ECD测定。对水样前处理和色谱条件等进行了优化选择。结果：本方法有机磷、拟除虫菊酯在0.05～1.0μg╱mL，有机氯在0.01～0.2μg／mL浓度范围内有良好的线性，方法检出限为0.0021～0.032μg／L(其中有机磷0.011～0.032μg／L，有机氯0.0021～0.0036μg／L，拟除虫菊酯0.0047～0.015μg╱L)。样品平均加标回收率在70.2％～104.0％，精密度以平行样品的相对标准差(RSD)表示，为2.2％～13.0％。结论：本方法具有操作简单、准确、灵敏、重现性好，安全环保等优点，适用于饮用水中部分拟除虫菊酯、有机氯及有机磷的检测。
Objective A multiresidue method based on solid-phase extraction andgas chromatography with electron capture detector was developed for thesimultaneous determination of 15 pesticides (Dichlorvos, Dimethoate,Parathion-methyl, Malathion, Parathion, Fenpropathrin, Lambda-cyhalothrin,Cypermethrin,Esfenvalerate,Deltamethfin,Quintozene,Dieldrin,Heptachlor,α-Endosulfan,β-Endosulfan) in drinking water. Method The extraction procedure was carried out in ENVI-C_(18) columnspreconditioned with methanol and water. The subsequent elution of pesticideswas performed with a mixture of acetone- hexane (25:75, v/v) prior to thedetermination by gas chromatography with electron capture detector, therecoveries of pyrethroids were remarkably increased by rinsing the containercontaining the sample with 5mL elution. Result Average recoveries for all the pesticides studied were higher than70% and relative standard deviations were below 13 % in the concentrationrange of 0.05～1.0μg/mL for organophosphorous and pyrethroids, 0.01～0.2μg/mL for organochlorine, the method showed good linearity ranges for allpesticides with correlation coefficients greater than 0.996. the detection limitsachieved ranged from 0.0021～0.032μg/L. Conelusion This method was simple,rapid,sensitive,accurate and safefor determination multiresidue of pesticides in drinking water.
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