液相色谱-串联质谱法测定大蒜中40种农药残留  

LC-MS/MS Determination of 40Pesticide Residues in Garlic

作　　者：王璐[1] 罗铭[1] 贺泽英[1] 彭袆[1] 刘潇威[1] 

机构地区：[1]农业部环境保护科研监测所,天津300191

出　　处：《理化检验（化学分册）》2015年第12期1702-1707,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：采用液相色谱-串联质谱法同时测定大蒜中40种农药的残留量。样品经磷酸酸化的乙腈提取后,采用QuEChERS方法净化,净化液采用Waters HSS T3C_(18)色谱柱分离,以甲酸-氨水-水(0.01+0.05+99.94)混合溶液和甲醇的混合液为流动相进行梯度洗脱,质谱中选择电喷雾电离源和多反应监测模式。40种农药的质量浓度均在5.0~400μg·L^(-1)范围内与峰面积呈线性关系,测定下限(10S/N)在0.1~5μg·kg^(-1)之间。加标回收率在70.1%~129%之间,测定值的相对标准偏差(n=5)在0.6%~9.3%之间。LC-MS/MS was applied to simultaneous determination of residual amounts of 40 pesticides in garlic.The sample was extracted with H_3PO_4-acidified acetonitrile and then purified by QuEChERS method.The purified solution was separated on Waters HSS T3C_（18） chromatographic column,using a mixture of methanol and HCOOH-NH4OH（0.01＋0.05＋99.94）solution as mobile phase in the gradient elution.ESI and MRM were adopted in MS.Linear relationships were found between values of peak areas and mass concentrations of the 40 pesticides in the same range of 5.0-400μg·L^（-1）,with lower limits of determinaiton（10S/N）in the range of0.1-5μg·kg^（-1）.Values of recovery obtained by standard addition method were in the range of 70.1%-129%,and RSDs found（n=5）were in the range of 0.6%-9.3%.

关 键 词：液相色谱-串联质谱法 农药残留 大蒜 

分 类 号：O657.63[理学—分析化学]