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气相色谱-质谱大体积进样法测定蔬菜、水果中17种农药残留
引用本文:黄惠玲, 张薇君, 丁慧瑛. 气相色谱-质谱大体积进样法测定蔬菜、水果中17种农药残留[J]. 分析测试学报, 2006, 25(4): 81-83,87
作者姓名:黄惠玲   张薇君   丁慧瑛
作者单位:1. 海南出入境检验检疫局,技术中心,海南,海口,570105
2. 浙江出入境检验检疫局,技术中心,浙江,杭州,310012
摘    要:建立了GC—MS/SIM与大体积进样技术结合测定蔬菜、水果中包括有机磷类、氨基甲酸酯类、有机氯类、菊酯类在内的17种农药的方法。样品经丙酮提取,OASIS HLB固相萃取小柱净化后,采用GC—Ms的选择离子模式和大体积进样技术进行测定,能够使相对检出限降低1~2个数量级。大多数农药的线性范围为0.05~10mg/kg,相关系数为0.9943—0.9996,相对标准偏差为3.5%-10.3%,回收率范围在77%~107%之间.方法能满足果蔬中17种农残限量的的检测要求,具有灵敏、快速、重复性好的特点。

关 键 词:气相色谱-质谱  大体积进样法  农药残留  蔬菜  水果
文章编号:1004-4957(2006)04-0081-03
收稿时间:2005-07-25
修稿时间:2005-07-252006-02-14

Determination of 17 Pesticide Residues in Vegetables and Fruits by Gas Chromatography- Mass Spectrometry with Large Volume Injection
HUANG Hui-ling,ZHANG Wei-jun,DING Hui-ying. Determination of 17 Pesticide Residues in Vegetables and Fruits by Gas Chromatography- Mass Spectrometry with Large Volume Injection[J]. Journal of Instrumental Analysis, 2006, 25(4): 81-83,87
Authors:HUANG Hui-ling  ZHANG Wei-jun  DING Hui-ying
Affiliation:1. Technological Center, Hainan Entry- Exit Inspection and Quarantine Bureau, Haikou 570105, China; 2. Technological Center, Zhejiang Entry -Exit Inspection and Quarantine Bureau, Hangzhou 310012, China
Abstract:A Method for the determination of 17 pesticides residues, including organophosphate, carbamate, prethroid in vegetables and fruits by gas chromatography - mass spectrometry with large volume injection.has been established. Samples were extracted with acetonitrile and then cleaned up by the OASIS HLB cartridge. The measurement was performed with the aid of gas chromatography - mass spectrometry in the selective ion monitoring mode with large volume injection. In comparison with conventional methods, the detection limits have been improved by 1 -2 orders of magnitude. The linear ranges for most pesticides were 0. 05 - 10 mg/kg while the correlation coefficient, relative standard deviation, and recoveries are 0. 994 3 -0. 999 6, 3.5% - 10. 3% and 77% - 107% , respectively. The method is suitable for the determination of 17 pesticide residues and is simple, rapid, accurate and practical.
Keywords:Gas chromatography - mass spectrometry   Large volume injection   Pesticide residues   Vegetables    Fruits
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