QuEChERS-UPLC-MS/MS法快速筛查稻米和稻茎中42种农药残留
投稿时间：2019-05-06      点此下载全文 HTML
引用本文：李亚辉,姚春霞,周佳欣,等.QuEChERS-UPLC-MS/MS法快速筛查稻米和稻茎中42种农药残留[J].农药学学报,2019,21(4):483-491.
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李亚辉 上海海洋大学 食品学院, 上海 201306
上海市农业科学院 农产品质量标准与检测技术研究所, 上海 201403 		 
姚春霞 上海市农业科学院 农产品质量标准与检测技术研究所, 上海 201403 67749801@qq.com 
周佳欣 上海市农业科学院 农产品质量标准与检测技术研究所, 上海 201403 45028338@qq.com 
孙小淋 上海市农业科学院 生态环境保护研究所, 上海 201403  
曹月琴 上海市闵行区农业技术服务中心, 上海 201101  
基金项目:沪农科推字（2018）第1-5号；上海市科委项目（17712400800，16391900500）；上海市崇明区科委攻关项目（CKS2018-12）
中文摘要:建立了QuEChERS前处理技术结合超高效液相色谱-串联质谱（UPLC-MS/MS）同时检测稻米和稻茎中42种农药残留的分析方法。样品经乙腈涡旋提取、QuEChERS净化管净化，C18超高效液相色谱柱分离后，在电喷雾正离子（ESI+）模式下，通过多反应监测正离子模式进行检测，采用基质匹配标准曲线峰面积外标法进行定量分析。结果表明：在0.01~0.2 mg/L范围内，42种农药的质量浓度与对应的峰面积间线性关系良好，R2 > 0.99，检出限为0.001~0.002 mg/kg。在0.01、0.02、0.05、0.1和0.2 mg/kg 5个添加水平下，42种农药在稻米和稻茎中的平均回收率均为70%~117%，相对标准偏差（RSD）稻米为1.5%~15%和稻茎为0.9%~15%。该方法具有操作简单、快速、灵敏度高、准确度高等优点，适用于稻米和稻茎中多种类农药残留的快速筛查分析。
中文关键词:QuEChERS  超高效液相色谱-串联质谱  稻米  稻茎  农药多残留  甲胺磷  甲霜灵  丙草胺
 
Rapid screening of 42 pesticides in rice and rice stems by QuEChERS-UPLC-MS/MS
Abstract:A method for the analysis of 42 pesticide residues in rice and rice stems was developed using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with QuEChERS pretreatment technology. The sample was extracted with acetonitrile vortex extraction, purified by QuEChERS purification tube and separated by C18 ultra-high performance liquid chromatography column. 42 analytes were measured under multiple reaction monitoring (MRM) using the electrospray positive ionization mode (ESI+). Quantification determination was performed by peak area external standard methods using matrix-matched calibration, which were linear in the range of 0.01-0.2 mg/L with good linear relationships. The determination coefficients (R2) were all above 0.99. The limits of detection (LOD) were lower than 0.002 mg/kg. The average recoveries of 42 pesticides in rice and rice stems all ranged from 70%-117%, and the relative standard deviations were in the range of 1.5%-15% in rice, and 0.9%-15% in rice stems, at the spiked levels of 0.01, 0.02, 0.05, 0.1 and 0.2 mg/kg. This method is simple, rapid, sensitivite, accuracy, which can be used in the simple and rapid screening of pesticide multi-residues in rice and rice stems.
Key words:QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  rice  rice stems  multi-residues of pesticides  methamidophos  metalaxyl  pretilachlor
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