气相色谱串联质谱法测定黄芪和西洋参中19种禁用农药  

Determination of 19 banned pesticides in Astragalus and American ginseng by gas chromatography tandem mass spectrometry

作　　者：常利民 汪春明 施鹏斐 杨波 张洋[1] 陈小同 王龙静 蒋文菊 张海江 CHANG Limin;WANG Chunming;SHI Pengfei;YANG Bo;ZHANG Yang;CHEN Xiaotong;WANG Longjing;JIANG Wenju;ZHANG Haijiang(Chinese Academy of Inspection and Quarantine Comprehensive Test Center,Beijing,100123,China;Beijing Bridge Technology Deveiopment Co.,Ltd.)

机构地区：[1]中国检验检疫科学研究院综合检测中心,北京100123 [2]北京新桥技术发展有限公司

出　　处：《质量安全与检验检测》2023年第2期6-16,共11页QUALITY SAFETY INSPECTION AND TESTING

摘　　要：本研究建立了HLB固相萃取与气相色谱串联质谱结合测定黄芪、西洋参中19种禁用农药的方法。试样经匀浆提取,HLB固相萃取柱净化,净化液经PTFE(polytetrafluoroethylene)有机相膜过滤后上机检测。GC-MS/MS方法以高纯氦气为载气,程序升温为:60℃,保持1 min,以30℃/min升至120℃,再以10℃/min升至160℃,再以2℃/min升至230℃,最后以15℃/min升至300℃,保持6 min;采用DB-17 MS(30 m×0.25 mm×0.25μm)色谱柱进行分离,离子源为电子轰击源(electron impact ion source,EI);多反应(multiple reaction monitoring,MRM)模式监测,基质匹配内标标准曲线法定量。结果显示,在0.003~0.200μg/mL质量浓度与其对应的峰面积之间线性关系良好,R^(2)均大于0.995,在0.01、0.02和0.05 mg/kg 3个添加水平下,禁用农药的平均回收率为61.9%~115.1%,相对标准偏差在1.0%~9.6%之间。表明HLB固相萃取法在保证净化效果和回收率的同时,能够满足禁用农药残留测定的需求,为快捷高效地测定黄芪、西洋参中19种禁用农药残留提供依据。In this study,a method for the determination of 19 banned pesticides in Astragalus and American ginseng by HLB solid phase extraction combined with gas chromatography-tandem mass spectrometry was established.The samples were extracted by homogenate,purified by HLB solid phase extraction column,and the purified liquid was filtered by PTFE organic membrane and then tested on the machine.The GC-MS/MS method uses high-purity helium as the carrier gas,and the program temperature is:60℃,hold for 1 min,increase to 120℃at 30℃/min,then increase to 160℃at 10℃/min,and then increase the temperature at 2℃/min to 230℃,and finally 15℃/min to 300℃,keep for 6 min;use DB-17 MS(30 m×0.25 mm×0.25μm)chromatographic column for separation,ion source is electron bombardment source(EI);multiple reaction(MRM)mode monitoring,matrix-matched internal standard standard curve method for quantification.Using Astragalus and American ginseng as the matrix,HLB solid phase extraction column purification,gas chromatography tandem mass spectrometry measured:the linear relationship between the mass concentration of 0.003-0.200μg/mL and the corresponding peak area is good,R^(2)is greater than 0.995,in 0.01,0.02 and 0.05 mg/kg 3 addition levels,the average recovery rate of banned pesticides is 61.9%-115.1%,and the relative standard deviation is between 0.7%-9.6%.The HLB solid phase extraction method is the preferred method.Whether it is purification effect or recovery rate,it can simultaneously meet the needs of determination of banned pesticide residues and provide a basis for the rapid and efficient determination of 19 banned pesticide residues in Astragalus and American ginseng.

关 键 词：黄芪 西洋参 19种禁用农药 QUECHERS 固相萃取 气相色谱-串联质谱法 

分 类 号：S481.8[农业科学—农药学] O657.63[农业科学—植物保护]