高效液相色谱-四极杆/静电场轨道阱高分辨质谱用于葡萄酒中111种农药残留的定性筛查与定量分析  

Screening and Quantification of 111 Pesticide Residues in Wines by High Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High-resolution Mass Spectrometry

作　　者：柳菡[1] 张亚莲[2] 丁涛[1] 王岁楼[2] 徐牛生 桂茜雯[1] 沈伟健[1] 赵增运[1] 吴斌[1] 沈崇钰[1] 张睿[1] 

机构地区：[1]江苏出入境检验检疫局动植物与食品检测中心,江苏南京210001 [2]中国药科大学药学院,江苏南京210009 [3]赛默飞世尔科技色谱质谱部,上海201206

出　　处：《分析测试学报》2014年第5期489-498,共10页Journal of Instrumental Analysis

基　　金：国家质量监督检验检疫总局科技计划项目(2011KJ39;2012KJ31);科技部科技支撑项目(2011BAK10B04)

摘　　要：建立了高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查和分析葡萄酒中多种农药残留的方法.葡萄酒样品经含0.1％醋酸的乙腈溶液提取,盐析后浓缩,甲醇水定容后,经N-丙乙二胺粉（PSA）净化,以C18柱为分析色谱柱,乙腈和5mmol/L醋酸铵水溶液为流动相进行梯度洗脱,使用高分辨质谱Q-Exactive采集数据.检测数据表明,111种农药在1～100 μg/L范围内线性关系良好,相关系数（r2）大于0.99.通过加标验证,该方法检出限可达到5μg/kg,回收率为63.3％～123.7％,RSD为3.2％A fast and easy method for the screening and quantification of 111 pesticides residues in wines by liquid chromatography - Quadrupole/Orbitrap high-resolution mass spectrometry was developed. ＂The wine samples were extracted with acetonitrile （containing 0. 1% acetic acid）, and salted out with anhydrous magnesium sulphate and anhydrous sodium acetate. After concentration, the analyte was dissolved with methanol and water, then cleaned up with primary secondary amine （PSA） to reduce matrix interference. Chromatographic analysis was carried out using a Cls column with acetoni- trile -5 mmol/L ammonium acetate solution as mobile phase by gradient elution. 111 pesticides residues were analyzed by high-resolution mass spectrometry in positive mode. Accurate mass extraction of the target pesticide compounds and data dependence threshold - triggered matrices interference during the analysis. The linearities of all 111 pesticides 100μg/L with correlation coefficients greater than 0. 99. By detecting Spiked samples, the limits ofdetection of the method were 5 μg/kg for all the pesticides residues and the recoveries were in the range of 63.3% - 123.7% with RSDs of 3.2% - 18.8%. This method could be used for highthroughput screening and confirmation of multiple pesticide residues in wines.

关 键 词：高效液相色谱 静电场轨道阱质谱 高分辨质谱 农药残留 葡萄酒 高通量 

分 类 号：O657.63[理学—分析化学]