高效液相色谱-电喷雾电离串联质谱法同时测定大豆..doc

高效液相色谱-电喷雾电离串联质谱法同时测定大豆中167种农药残留 陈树兵*，钟莺莺，贺小雨，樊苑牧 （宁波出入境检验检疫局技术中心，浙江 宁波，315012） 摘要：建立了高效液相色谱-电喷雾电离源串联质谱同时测定大豆中167种农药残留。样品用乙腈提取，盐析分层后，经C18、PSA固相萃取柱净化后，再用高效液相色谱-电喷雾电离串联质谱法在正负离子切换多反应检测模式（MRM）下测定，基质曲线外标法定量。167种农药在大豆中3个添加水平的平均回收率为67.3-123.5%，相对标准偏差为4.7-13.9%。基质标准曲线在0-50.0 ng/mL浓度范围内线性关系良好，相关系数均大于0.99，最低添加浓度0.01mg/kg作为方法定量限（S/N远大于10）。本方法检测通量高、定量限低、准确度和精密度符合要求，适用于大豆中多种农药残留的筛查定量分析。 关键词：高效液相色谱-串联质谱；大豆；农药多残留 Simultaneous Determination of 167 Pesticide Residues in Soybean by Liquid Chromatography-Electrospray Tandem Mass Spectrometry Chen Shubing, Zhong Yingying, He Xiaoyu, Fan Yuanmu (Technology Center of Ningbo Entry-Exit Inspection and Quarantine Bureau, Ningbo 315012, China) Abstract：A method was developed for simultaneous determination of 167 pesticide residues in soybean by liquid chromatography-electrospray tandem mass spectrometry (LC-MS/MS). Sample was extracted with acetonitrile, followed by salting out. The extract was purified with C18 and PSA solid phase extraction columns, and analyzed by LC-MS/MS in either positive or negative multi reaction mode and calculated with matrix-match standard solutions as external standard. The average recoveries were 67.3-123.5% for spiked samples in three different concentrations，with RSD between 4.7% and 13.9%. The calibration curves of all pesticides were linear in the range of 0-50 ng/mL with the correlation coefficient more than 0.99. The lowest spiked concentration was used as the quantitation limit where the S/Ns for all pesticides were more than 10. The proposed method was suitable for screen of multi-pesticide residues in soybean for its high sample throughput, low LOQ, good accuracy and precision. Key words：LC-MS/MS；soybean；multi-pesticide residues 随着国外大豆进口量的逐年增加，我国已经从大豆净出口国变成了世界上最大的大豆进口国。近年来，检验检疫部门曾多次在进口大豆中检出含萎锈灵、福美双、甲霜灵等种衣剂农药残留，进口大豆农药残留问题引起了越来越多的关注。世界各国和国际组织对大豆中农药残留的限量标准所规定的项目各不相同，我国《食品安全国家标准 食品中农药最大残留限量 目前，国内已有的关于大豆中的农药残留分析方法主要有采用色谱或色谱-质谱法2-4] 测[定几种或一类农药残留，大豆中高通量、高灵敏度的多种农药残留检测的方法还未见报道。本方法利用液相色谱-串联质谱具有的灵敏、准确、抗干扰能力强的优势，建立