液相色谱_串联质谱法同时测定中药材中74种农药残留量.pdfVIP

液相色谱 串联质谱法同时测定中药材中 74种农药残留量 毛秀红 ,郏征伟 ,陈钶 ,王柯 ,季申 (上海市食品药品检验所 ,上海 20 1203) ( ) 摘要 : 目的　研究中药材中农药多残留的测定方法 。方法 　样品经加速溶剂萃取 ,依次经凝胶渗透色谱 GPC 和固相萃取柱 ( ) SPE 净化后 ,用液相色谱 串联质谱同时定性 、定量测定 。结果 　在 6种中药材样品基质 、3水平添加条件下 , 74 种农药的回 收率大多在 700% ～1100% ,相对标准偏差小于 15% ,检测限大多低于 00 1 m g ·kg- 1 ,符合农药多残留检测的要求 。结论 　本法净化效果好 ,灵敏度高 ,重现性好 ,可用于中药材样品中农药多残留的日常检测 。 关键词 : 中药材 ;农药残留;加速溶剂萃取 ;凝胶渗透色谱 ; 固相萃取 ;液相色谱 串联质谱法 中图分类号 : R9 17　　　文献标识码 : A 　　　文章编号 : 100 1 - 2494 (20 10) 0 1 - 0064 - 07 S im ultaneous D eterm ina tion of 74 Pestic ides in Trad itiona l Ch ine se Herba l M ed ic ines by L C M S /M S MAO X iu hong, J IA Zhengwei, CH EN Ke, WAN G Ke, J I Shen (D ep a rtm en t of Trad itiona l Ch ineseM ed icine, S hangha i Ins titu te f or F ood and D rug Con trol, S hang ha i 20 1203, Ch ina) A BSTRACT :O BJECT IVE　To study the m u ltire sidues m ethod s for traditional Ch inese herbal m edicine s ( TCHM s) M ETHOD S　 74 Pe sticide s were extracted by accelerated so lvent extraction, and then p urified w ith gel p erm eation chrom atography ( GPC) and so lid p hase extraction ( SPE) cartridge s The residue s were simu ltaneou sly identified and quantified by LCM S/M S RESUL TS　The ana lytical p erform ance wa s demon strated by the analysis of 6 TCHM s samp le s extracts, sp iked at three concentration levels for each p esti cide The recoverie s ranged from 70% to 110% , w ith relative standard deviation s ( R SD s) above 15% The lim it of quantification (LOD ) for mo st of the targeted p esticides wa s below 00 1 m g ·kg- 1 CO NCL US IO N　The m ethod had the good extraction efficien cy and p urification effect, wh ich cou ld be app lied to the determ ination of p esticide residue s in the rou tine analysis of TCHM s KEY W O