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液相色谱-串联质谱法检测黄瓜中5种有机磷农药残留
引用本文:王雯,梁颖,沈燕,马尧瑶,钱建亚,刘贤进.液相色谱-串联质谱法检测黄瓜中5种有机磷农药残留[J].南京农业大学学报,2012,35(1):45-50.
作者姓名:王雯  梁颖  沈燕  马尧瑶  钱建亚  刘贤进
作者单位:1. 江苏省食品质量安全重点实验室,江苏南京210014;扬州大学食品科学与工程学院,江苏扬州225009
2. 江苏省食品质量安全重点实验室,江苏南京210014;农业部食品安全监控重点开放实验室,江苏南京210014
3. 江苏省食品质量安全重点实验室,江苏南京,210014
4. 扬州大学食品科学与工程学院,江苏扬州,225009
基金项目:江苏省自主创新资金项目
摘    要:建立液相色谱-串联质谱(LC-MS/MS)同时检测黄瓜中敌百虫、乐果、敌敌畏、杀螟硫磷、毒死蜱5种有机磷农药残留的方法。样品经过丙酮提取,弗罗里硅土净化,以甲醇-水(水相含0.1%甲酸)为流动相梯度洗脱,采用ZORBAX SB-C18(5μm×2.1 mm×150 mm)色谱柱分离,电喷雾离子化正模式(ESI+)离子化,多反应监测模式(MRM)下测定。结果显示:方法标准曲线线性良好,R2≥0.998;乐果与敌敌畏的定量限为0.002 mg.kg-1,敌百虫、杀螟硫磷和毒死蜱的定量限为0.01mg.kg-1;回收率为72%~98%,相对标准偏差(RSD)≤3.6%。表明:该方法可实现对5种有机磷农药的同时快速测定,目标农药的响应值高,检测限低,能够为生食蔬菜风险评估研究提供准确有效的数据支持。

关 键 词:液相色谱-串联质谱  有机磷农药  黄瓜  检测

Simultaneous determination of five organophosphorus pesticide residues in cucumber by LC-MS/MS
WANG Wen , LIANG Ying , SHEN Yan , MA Yao-yao , QIAN Jian-ya , LIU Xian-jin.Simultaneous determination of five organophosphorus pesticide residues in cucumber by LC-MS/MS[J].Journal of Nanjing Agricultural University,2012,35(1):45-50.
Authors:WANG Wen  LIANG Ying  SHEN Yan  MA Yao-yao  QIAN Jian-ya  LIU Xian-jin
Institution:1,3(1.Key Laboratory of Food Quality and Safety,Jiangsu Province,Nanjing 210014,China;2 College of Food Science and Engineering,Yangzhou University,Yangzhou 225009,China;3.Key Laboratory of Food Safety Monitoring and Management,Ministry of Agriculture,Nanjing 210014,China)
Abstract:A method to identify and quantify five organophosphorus pesticides about trichlorfon,dimethoate,dichlorvos,fenitrothion and chlorpyrifos in cucumber was developed using the liquid chromatography-tandem triple quadrupole mass spectrometric(LC-MS/MS).The sample was extracted by acetone and cleaned up with florisil.The separation was performed on a ZORBAX SB-C18(5 μm×2.1 mm×150 mm)with the gradient elution of methanol-water with 0.1% formic acid(volume ratio)as mobile phase.Sample was detected by multiple reaction monitoring(MRM)with electric spray ionization(positive).The result showed that satisfactory linear results have been got with R2≥0.998.The limit of quantity(LOQ)of dimethoate and dichlorvos was 0.002 mg·kg-1,and the limit of quantitaty(LOQ)of trichlorfon,fenitrothin and chlorpyrifos was 0.01 mg·kg-1,depending on the matrices and spiked concentration,ranging from 72% to 98% with relative standard deviations(RSD)≤3.6%.This simple,rapid and sensitive method can be applied to supplying reliable data for the study of the risk assessment of raw vegetables.
Keywords:liquid chromatography-tandem triple quadrupole mass spectrometric(LC-MS/MS)  organophosphorus pesticide  cucumber  determination
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