气相色谱-质谱法测定茶叶中溴虫腈、啶虫脒、茚虫威、三氯杀螨醇及拟除虫菊酯等11种农药残留  

Determination of 11 pesticide residues,such as chlorfenapyr,acetamiprid,indoxacarb,dicofol and synthetic pyrethroids in tea by gas chromatography-mass spectrometry

作　　者：李晔[1] 郭蒙京[1] 袁佗[1] 

机构地区：[1]北京市西城区疾病预防控制中心,北京100120

出　　处：《中国卫生检验杂志》2016年第11期1579-1581,1584,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立茶叶中溴虫腈、啶虫脒、茚虫威、三氯杀螨醇及拟除虫菊酯类等11种农药的气相色谱-质谱(GCMS)分析方法。方法采用乙腈萃取待测组分,萃取液经过氮吹浓缩至1 ml左右;固相萃取净化后,样品经过DB-17MS毛细管色谱柱程序升温分离,质谱选择离子监测模式(SIM)检测,外标法定量。结果所测11种农药的浓度为0.05 mg/L^10 mg/L时,线性关系良好,相关系数(r)≥0.997 3,平均回收率为72%~114%,相对标准偏差≤16.7%。方法的检出限(LOD)为0.001 mg/kg^0.01 mg/kg,定量限(LOQ)为0.004 mg/kg^0.040 mg/kg。结论方法简单、准确、灵敏度高,适用于茶叶中农药多残留同时检测的要求。Objective An analytical method was developed for the determination of 11 pesticides,such as chlorfenapyr,acetamiprid,indoxacarb, dicofol and synthetic pyrethroids in tea by gas chromatography-mass spectrometry（ GC / MS）.Methods After extracted with acetonitrile,samples were concentrated to 1 ml with blowing nitrogen,and then cleaned up by solid phase exaction,the samples were separated by DB-17 MS column using programmed temperature. MS was conducted in ion monitoring mode（ SIM） for detection,and external standard method was used for quantification. Results The method showed a good linearity（ r≥0. 997 3） in the ranges of 0. 05 mg / L-10 mg / L for 11 pesticide with average recovery rates among72%-114% and the relative standard deviation（ RSD） ≤16. 7%. The limits of detection（ LODs） were among 0. 001 mg / kg-0. 01 mg / kg,and the limits of quantification（ LOQ） was among 0. 004 mg / kg-0. 040 mg / kg. Conclusion The method is simple,sensitive,accurate and is suitable for the simultaneous detection of multi-residue pesticides in tea.

关 键 词：气相色谱-质谱法 农药残留 茶叶 

分 类 号：O657.63[理学—分析化学]