气相色谱-质谱法测定水产品中硫丹和毒死蜱的残留量
GC-MS Determination of Residual Endosulfan and Chlorpyrifos in Aquatic Products
摘 要
提出了气相色谱四极杆质谱法测定鳗鱼中硫丹和毒死蜱农药残留量的方法.样品以乙酸乙酯为提取剂,经浓缩、净化、氮气吹干后用正己烷溶解,采用气相色谱-质谱负化学电离源方式进行选择离子扫描测定.各标准曲线线性范围为0.2~10.0 μg·kg-1,回收率为81%~95%;测定结果的相对标准偏差(n=8)小于5%,检出限(3S/N)为0.5 μg·kg-1.
农药残留
测定
水产品
硫丹
毒死蜱
GC-MS
Residual pesticide
Determination
Aquatic products
Endosulfan
Chlorpyrifos
Abstract
Residual amounts of endosulfan and chlorpyrifos in aquatic products (taking eel as testing sample) were determined by GC-MS with negative chemical ionization (NCl) source.The smashed and slurried sample was extracted with ethyl acetate,and the extract obtained was evaporated to dryness at 40 ℃.The residue was taken up with acetonitrile and purified by passing through the acidic aluminum oxide chromatographic column,and the acetonitrile solution was dried at 50 ℃ by N2-blowing.The dried residue was dissolved in a definite volume of n-hexane and used for GC-MS determination with SIM mode.Ranges of linearity of standard curves for the 3 compounds (i.e.,chlorpyrifos,α-endosulfan and β-endosulfan) found were all in the range of 0.2 μg·kg-1 to 10.0 μg·kg-1.Detection limit (3S/N) of the method was found to be 0.5 μg·kg-1.Values of recovery found were in the range of 81%-95%,and values of RSD′s (n=8) were less than 5%.
中图分类号 O657.31
所属栏目 工作简报
基金项目
收稿日期 2007/8/19
修改稿日期
网络出版日期
作者单位点击查看
备注高华鹏(1977-),男,宁波人,工程师,从事食品检测工作.
引用该论文: GAO Hua-peng,YU Xue-jun,SHEN Wei-jun,LI Yong-fu,LI Zuo-qing. GC-MS Determination of Residual Endosulfan and Chlorpyrifos in Aquatic Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(1): 85～87
高华鹏,俞雪均,沈维军,李永夫,李佐卿. 气相色谱-质谱法测定水产品中硫丹和毒死蜱的残留量[J]. 理化检验－化学分册, 2009, 45(1): 85～87
共有人对该论文发表了看法，其中：
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】明九雪,钱传范,申继忠.硫丹在苹果和土壤中的残留动态研究[J].中国农业大学学报,1998,3(3):95-100．
【2】Arrebola F J,Martinez vidal J L,Fernandez-guterrez A.Analysis of endosulfan and its metabolites in human serum using gas chromatography-tandem mass spectrometry[J].J Chrom Sci,2001,39(5):177-182．
【3】Martinez vidal J L,Arrebola F J,Fernandez-guterrez A,et al.Determination of endosulfan and its metabolites in human urine[J].J Chromatog B,1998,19:71-78．
【4】林竹光,金珍,马玉,等.气相色谱-质谱法分析蜂蜜中多种有机氯农药残留[J].分析试验室,2006,25(6):12-17．
【5】余建新,邵俊杰,胡小钟,等.水果、蔬菜中16种有机氯残留农药的毛细管气相色谱测定法[J].分析测试学报,1999,18(3):29-31．
【6】王建,贾斌,林秋萍,等.气相色谱-质谱联用法确证蔬菜中多种农药残留[J].理化检验-化学分册,2006,42(7):533-535．
【7】张均媚,薛刚,刘伟娟.气相色谱-质谱法测定茶叶中12种农药残留的方法[J].食品研究与开发,2005,26(3):157-159．
【8】吴刚,虞慧芳,鲍晓霞,等.茶叶种杀螟丹残留的气相色谱分析方法研究[J].中国食品学报,2006,6(5):129-132．
【9】郝丽丽,薛健.银杏叶中18种有机氯农药的多残留分析[J].分析化学,2006,34(2):231-234．
【10】沈崇钰,沈伟健,蒋原,等.气相色谱-负化学源质谱联用法测定菊酯类农药[J].分析化学,2006,36:36-40．
【11】王微国,李重九,李玉兰,等.有机质谱应用-在环境、农业和法庭科学中的应用[M].北京:化学工业出版社,2005:95．
【2】Arrebola F J,Martinez vidal J L,Fernandez-guterrez A.Analysis of endosulfan and its metabolites in human serum using gas chromatography-tandem mass spectrometry[J].J Chrom Sci,2001,39(5):177-182．
【3】Martinez vidal J L,Arrebola F J,Fernandez-guterrez A,et al.Determination of endosulfan and its metabolites in human urine[J].J Chromatog B,1998,19:71-78．
【4】林竹光,金珍,马玉,等.气相色谱-质谱法分析蜂蜜中多种有机氯农药残留[J].分析试验室,2006,25(6):12-17．
【5】余建新,邵俊杰,胡小钟,等.水果、蔬菜中16种有机氯残留农药的毛细管气相色谱测定法[J].分析测试学报,1999,18(3):29-31．
【6】王建,贾斌,林秋萍,等.气相色谱-质谱联用法确证蔬菜中多种农药残留[J].理化检验-化学分册,2006,42(7):533-535．
【7】张均媚,薛刚,刘伟娟.气相色谱-质谱法测定茶叶中12种农药残留的方法[J].食品研究与开发,2005,26(3):157-159．
【8】吴刚,虞慧芳,鲍晓霞,等.茶叶种杀螟丹残留的气相色谱分析方法研究[J].中国食品学报,2006,6(5):129-132．
【9】郝丽丽,薛健.银杏叶中18种有机氯农药的多残留分析[J].分析化学,2006,34(2):231-234．
【10】沈崇钰,沈伟健,蒋原,等.气相色谱-负化学源质谱联用法测定菊酯类农药[J].分析化学,2006,36:36-40．
【11】王微国,李重九,李玉兰,等.有机质谱应用-在环境、农业和法庭科学中的应用[M].北京:化学工业出版社,2005:95．
相关信息
