QuEChERS-气相色谱-串联质谱法测定茶青中28种农药残留  

Determination of 28 pesticide residues in fresh tea leaves using QuEChERS-gas chromatography-tandem mass spectrometry

作　　者：李俊[1] 蔡滔[1] 杜楠[1] 周雪丽[1] 王震[1] 袁旭[1] 卢平[2] 陈玉玲[2] 

机构地区：[1]贵州省农产品质量安全监督检验测试中心/农业部农产品质量安全风险评估实验室(贵阳),贵阳550004 [2]贵州大学精细化工研究开发中心/教育部绿色农药与生物工程重点实验室,贵阳550025

出　　处：《农药学学报》2017年第3期366-373,共8页Chinese Journal of Pesticide Science

基　　金：黔科合重大专项字([2013]6024号);国家自然科学基金项目(21365007);国家农产品质量安全风险评估项目(GJFP2017005)

摘　　要：建立了QuEChERS-气相色谱-串联质谱(GC-MS/MS)同时测定茶青中28种农药残留的分析方法。样品采用乙腈匀浆提取,经75 mg PSA、25 mg C18、4 mg GCB净化,GC-MS/MS多反应离子监测模式下检测,外标法定量。结果表明:在0.020~0.40 mg/L范围内,28种农药的质量浓度与对应的峰面积间呈良好的线性关系,决定系数均大于0.991。在0.10和0.50 mg/kg两个添加水平下,28种农药的平均回收率在77%~106%之间,相对标准偏差(RSD)在1.4%~8.0%(n=6)之间。方法的检出限(LOD)为5.0~20μg/kg,定量限(LOQ)为10~60μg/kg。该方法简单、快速、准确、灵敏度高,可用于茶青中多种农药残留的同时检测分析。A multiresidue analytical method for the determination of 28 pesticide residues in fresh tea leaves was developed and evaluated by using QuEChERS （quick, easy, cheap, effective, rugged and safe） and triple-quadrupole tandem mass spectrometry （GC-MS/MS）. Samples were extracted by acetonitrile, and purified by 75 mg PSA, 25 mg C18 and 4 mg GCB, followed by GC-MS/MS detection under multi-reaction monitoring （MRM） mode and quantified by external standard method. Good linearity was achieved between area size and concentration from 0.020 to 0.40 mg/L, with a coefficient of determination higher than 0.991. The average recovery at different spiking levels （0.10, 0.50 μg/kg） was ranged from 77% to 106% with RSD （relative standard deviation, n = 6） 1.4%-8.0%. The LOD （limit of detection） was 5.0-20 μg/kg, and LOQ （the limit of quantification） was 10-60 μg/kg. The method was simple, quick, accurate, highly sensitive and suitable for the simultaneous analysis of multiresidues of pesticides in fresh tea leaves.

关 键 词：QUECHERS 气相色谱-串联质谱 茶青 农药 残留 

分 类 号：S481.8[农业科学—农药学] TQ450[农业科学—植物保护]