摘要
适量水浸润的铁皮石斛样品经乙腈高速涡旋和超声提取。离心后,上清液采用分散固相萃取净化,吸附剂为C18和N-丙基乙二胺。采用分散固相萃取-气相色谱-串联质谱法测定净化液中41种农药的残留量。在气相色谱分离中采用Agilent VF-5MS色谱柱,在串联质谱分析中采用多反应监测模式。以外环氧七氯为内标,41种农药的检出限(3S/N)为0.001～0.024 mg·kg^(-1)。以空白样品为基体进行加标回收试验,所得回收率为75.1%～115%,测定值的相对标准偏差(n=6)为0.40%～11%。
The dendrobium candidum sample soaked with appropriate amount water was extracted ultrasonically with acetonitrile accompanied by high speed vortex.After centrifugation,the supernatant was purified with dispersive solid phase extraction.C18 and PSA were used as adsorbents.GC-MS/MS was applied to the determination of residual amounts of 41 pesticides in purified liquid with dispersive solid phase extraction.Agilent VF-5 MS chromatographic column was used for GC separation and the multiple reaction monitoring mode was adopted in MS/MS determination.cis-Heptachlor epoxide was used as internal standard.Detection limits(3 S/N)of the 41 pesticides were in the range of 0.001-0.024 mg·kg-1.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 75.1%-115%,with RSDs(n=6)of determined values in the range of 0.40%-11%.
作者
周敏
朱萌萌
何晓明
孙文闪
刘芯成
王珍
ZHOU Min;ZHU Mengmeng;HE Xiaoming;SUN Wenshan;LIU Xincheng;WANG Zhen(Greentown Agricultural Testing Technology Co.,Ltd.,Hangzhou 310052,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2019年第2期162-170,共9页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
作者简介
周敏,工程师,主要从事食品检测工作,minzhou117@163.com.
