分散固相萃取-液相色谱-串联质谱法测定水果中19种酸性农药

建立了同时检测葡萄、苹果和桔子等水果中2,4-滴等19种酸性农药的分散固相萃取-液相色谱-串联质谱（HPLC-MS/MS）方法。葡萄、苹果和桔子样品经乙酸-乙腈（1∶99,V/V）提取后,C18分散固相萃取净化,采用反相C18色谱柱分离。以0.1%甲酸和0.1%甲酸-乙腈溶液作为流动相进行梯度洗脱,采用多反应监测离子模式进行定性分析,基质标准曲线外标法进行定量分析,线性范围在0.01~0.2 mg/kg之间。在0.02,0.05和0.1 mg/kg添加水平下,19种酸性农药的回收率为70.3%～105.3%;相对标准偏差为0.37%～10.9%。本方法的定量限为0.005～0.02 mg/kg...

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Published in分析化学 Vol. 41; no. 3; pp. 354 - 359
Main Author 金芬 史晓梅 于志勇 李敏洁 邵华 金茂俊 王静
Format Journal Article
LanguageChinese
Published 中国农业科学院农业质量标准与检测技术研究所农产品质量与食物安全重点实验室,北京,100081%中国科学院生态环境研究中心环境水质学国家重点实验室,北京,100085 2013
Subjects
分散固相萃取
水果
液相色谱-串联质谱
酸性农药
酸性农药
水果
液相色谱-串联质谱
分散固相萃取
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Summary:建立了同时检测葡萄、苹果和桔子等水果中2,4-滴等19种酸性农药的分散固相萃取-液相色谱-串联质谱（HPLC-MS/MS）方法。葡萄、苹果和桔子样品经乙酸-乙腈（1∶99,V/V）提取后,C18分散固相萃取净化,采用反相C18色谱柱分离。以0.1%甲酸和0.1%甲酸-乙腈溶液作为流动相进行梯度洗脱,采用多反应监测离子模式进行定性分析,基质标准曲线外标法进行定量分析,线性范围在0.01~0.2 mg/kg之间。在0.02,0.05和0.1 mg/kg添加水平下,19种酸性农药的回收率为70.3%～105.3%;相对标准偏差为0.37%～10.9%。本方法的定量限为0.005～0.02 mg/kg。
Bibliography:Liquid chromatography-tandem mass spectrometry; Acidic pesticides; Dispersive solid phase extraction; Fruit
JIN Fen , SHI Xiao-Mei , YU Zhi-Yong, LI Min-Jie, SHAO Hua, JIN Mao-Jun , WANG Jing （Key Lab of Agro-product Quality and safety, Institute of Quality Standards ＆ Testing Technology for Agro-products, Chinese Academy of Agricultural Sciences, Beijing 100081, China） 2 （State Key Laboratory of Environmental Aquatic Chemistry, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China）
22-1125/O6
A method was developed for the determination of 19 acidic pesticides in fruit by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry （LC-MS/MS）. The 19 analytes were extracted from the fruit samples by acetic acid-acetonitrile （1：99, V/V）, and purified by dispersion solid phase extraction using C18 sorbent, and then analyzed by liquid chromatography-tandem mass spectrometry （LC-MS/MS）. The 19 analytes were then separated on a reversed phase colum
ISSN:0253-3820
DOI:10.3724/SP.J.1096.2013.20750