气相色谱-质谱法测定蔬菜和水果中螺虫乙酯的残留量  被引量:13

GC-MS Determination of Residual Amount of Spirotetramat in Vegetables and Fruits

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作  者:郭庆龙[1] 管旭芳[1] 赵勇[1] 李瑞娟[2] 于建垒[2] 

机构地区:[1]黄岛出入境检验检疫局,青岛266555 [2]山东省农业科学院植物保护研究所,济南250100

出  处:《理化检验(化学分册)》2017年第8期885-889,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基  金:山东出入境检验检疫科研课题资助项目(SK201425)

摘  要:采用气相色谱-质谱法测定蔬菜和水果中螺虫乙酯的残留量。蔬菜或水果样品经乙腈均质提取,以乙二胺-N-丙基硅烷和十八烷基硅烷为基质分散固相萃取剂净化。在气相色谱分离中用HP-5MS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。螺虫乙酯的质量浓度在10~500μg·L^(-1)内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.75μg·kg^(-1),测定下限(10S/N)为2.51μg·kg^(-1)。以空白样品为基体进行加标回收试验,所得回收率为79.8%~101%,测定值的相对标准偏差(n=6)为4.1%~8.7%。GC-MS was applied to the determination of residual amount of spirotetramat in vegetables and fruits.The sample of vegetable or fruit was extracted with acetonitrile homogeneously,and purified by matrix dispersion solid phase extraction with PSA and C_(18).The HP-5MS capillary chromatographic column was used for GC separation and the selected ion monitoring mode was adopted in MS determination.Linear relationship between values of peak area and mass concentration of spirotetramat was kept in the range of 10-500μg·L^(-1),with detection limit(3S/N)of 0.75μg·kg^(-1) and lower limit of determination(10S/N)of 2.51μg·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 79.8%-101%,with RSD′s(n=6)in the range of 4.1%-8.7%.

关 键 词:气相色谱-质谱法 蔬菜 水果 螺虫乙酯 

分 类 号:O657.63[理学—分析化学]

 

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