摘要
叶菜类蔬菜种植土壤样品过筛(180μm)后,加入无水硫酸钠和硅藻土进行研磨,所得样品再以丙酮与正己烷以体积比2∶3组成的混合液为萃取溶剂进行加速溶剂萃取,萃取液用氮气吹至近干,净化后,采用气相色谱-串联质谱法测定净化液中啶虫脒、茚虫威、氯虫苯甲酰胺、辛硫磷、异菌脲等5种杀虫剂的残留量。在气相色谱分离中采用HP-5MS色谱柱,在串联质谱分析中采用多反应监测模式。5种杀虫剂的质量浓度均在0.05~5.0mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.010~0.018μg·kg-1。以空白土壤样品为基体进行加标回收试验,所得回收率为76.9%~100%,测定值的相对标准偏差(n=6)为1.5%~4.1%。
Sample of leafy vegetables growing soil obtained after sieving(180μm)was added with anhydrous sodium sulfate and diatomite to grind.The sample obtained by the above procedure was extracted with the mixture of acetone and n-hexane(volume ratio of 2∶3)used as extraction solvent for accelerated solvent extraction.The extract was evaporated to near dryness by N2-blowing.After purification,GC-MS/MS was applied to the determination of residual amounts of 5 pesticides,i.e.acetamiprid,indoxacarb,chlorantraniliprole,phoxim and iprodione in purified liquid.The HP-5 MS chromatographic column was used for GC separation and the multiple reaction monitoring mode was adopted in MS/MS determination.Linear relationships between values of peak area and mass concentration of the 5 pesticides were kept in the same range of 0.05-5.0 mg·L-1,with detection limits(3S/N)in the range of 0.010-0.018μg·kg-1.On the base of blank soil sample,test for recovery was made by standard addition method;values of recovery found were in the range of 76.9%-100%,with RSDs(n=6)of determined values in the range of 1.5%-4.1%.
作者
后小龙
张文锦
HOU Xiaolong;ZHANG Wenjin(Gansu Province Dingxi City Environmental Monitoring Station,Dingxi 743000,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2020年第7期822-826,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
