固相萃取-气相色谱-质谱法测定水果中9种菊酯农药残留量  

SPE-GC-MS Determination of Residual Amounts of 9Pyrethroid Pesticides in Fruits

作　　者：卢亚玲[1,2] 祝文君[1] 艾明艳[1] 刘文杰[1,2] 

机构地区：[1]塔里木大学生命科学学院,阿拉尔843300 [2]塔里木盆地生物资源保护利用兵团重点实验室,阿拉尔843300

出　　处：《理化检验（化学分册）》2015年第7期970-973,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：塔里木大学校长基金项目(TDZKSS201312)

摘　　要：采用固相萃取-气相色谱-质谱法测定水果中9种菊酯农药的残留量。水果样品经丙酮-水（5＋1）混合液匀质提取,二氯甲烷萃取,石墨碳柱净化。在气相色谱分离中用DB-5毛细管色谱柱为固定相,在质谱分析中采用选择离子监测模式。9种菊酯农药的质量浓度均在0.1-5mg·L^-1范围内与其峰面积呈线性关系,方法的检出限（3S/N）在0.000 6-0.01mg·kg^-1之间。方法用于水果样品的分析,加标回收率在75.0%-106%之间,测定值的相对标准偏差（n=5）在1.6%-4.2%之间。GC-MS was applied to the determination of residual amounts of 9pyrethroid pesticides in fruits after separation by solid phase extraction.The fruit sample was extracted homogeneously with acetone-H2O（5＋1）mixture,and the extract was further extracted with methylene chloride.The extract obtained was then purified on graphite carbon column.DB-5capillary chromatographic column was used for GC separation and selected ion monitoring mode was adopted in MS determination.Linear relationships between values of peak area and mass concentration of the 9pyrethroid pesticides were kept in the same range of 0.1-5mg·L^-1,with detection limits（3S/N）in the range of 0.000 6-0.01 mg·kg^-1.The proposed method was applied to the analysis of fruit samples,giving values of recovery and RSD′s（n=5）in the ranges of 75.0%-106% and 1.6%-4.2%respectively.

关 键 词：气相色谱-质谱法 固相萃取 菊酯农药 水果 

分 类 号：O657.63[理学—分析化学]