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投稿时间:2018-06-10
投稿时间:2018-06-10
中文摘要: 建立固相萃取-液相色谱串联质谱法同时检测蔬菜中28种农药残留的分析方法。样品经乙腈匀浆提取,盐析离心,NH2固相萃取柱净化,采用液相色谱分离,多反应监测(multiple reaction monitoring,MRM)模式进行检测,基质曲线外标法定量。啶虫脒的线性范围为7.5 ng/mL~300 ng/mL,其他农药的线性范围为5.0 ng/mL~200 ng/mL,线性相关系数均大于 0.996 8,28 种农药的定量限(limits of quantitation,LOQ)为 0.7 μg/kg~6.0 μg/kg。啶虫脒在 30、60、150 μg/kg 3 个添加水平,其他农药在20、40、100 μg/kg 3个添加水平下的回收率为63.9%~120.4%,相对标准偏差(relative standard deviations,RSD)为2.4%~9.8%。该方法适合同时检测不同品种蔬菜中的28种农药残留,能满足实验室的日常检测需求,具有实际应用意义。
中文关键词: 高效液相色谱-串联质谱 NH2固相萃取柱 蔬菜 农药残留
Abstract:An analytical method was developed for the simultaneous determination of 28 pesticide in vegetables based on solid phase extraction followde by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The samples were extracted using acetonitrile homogenate and centrifuged by salting,NH2solid phase extraction column purification.The target analytes were separated on HPLC column and analyzed in multiple reaction monitoring(MRM)mode.Sample matrix-matched calibration was used to determine the residue contents by external standard.The results showed that the calibrationcurves in the range of 7.5 ng/mL-300 ng/mL for acetamiprid,and 5.0 ng/mL-200 ng/mL for other pesticides,with correlation coefficients larger than 0.996 8.The limits of quantitation (LOQ)were of 28 pesticides 0.7 μg/kg-6.0 μg/kg.The recoveries of acetamiprid with the concentration levels at 30,60,150 μg/kg and other pesticides with the concentration levels at 20,40,100 μg/kg were range of 63.9%-120.4%,which relative standard deviations (RSD)were 2.4%-9.8%.This method was suitable for qualification of 28 pesticide in vegetables,meet the daily testing requirements of the laboratory and has practical application significance.
keywords: high performance liquid chromatography-tandem mass spectrometry(HPLC-MS-MS) NH2solid phase extraction vegetable foods pesticide residues
文章编号:201824026 中图分类号: 文献标志码:
基金项目:湖北省食品药品监督管理局科研项目(201601016)
Author Name | Affiliation |
YANG Yu-ping,TU Lin,JIN Chan,QIN Juan,LI Wen-bo,TANG Jing-miao,XIE Bai-yan | Wuhan Institute for Drug and Medical Device Control,Wuhan 430075,Hubei,China |
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