液相色谱-串联质谱法测定洋葱中灭多威和杀线威残留量  

LC-MS/MS Determination of Residual Amounts of Methomyl and Oxamyl in Onion

作　　者：倪永付[1] 朱涛[1] 闫秋成 

机构地区：[1]济宁出入境检验检疫局,济宁272000

出　　处：《理化检验（化学分册）》2017年第7期865-868,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：山东出入境检验检疫局科研项目(SK201426)

摘　　要：样品5.000 0g,加入乙腈10mL,无水硫酸钠5g,混匀,涡旋振荡提取30min。提取液2mL经石墨烯(14mg)分散固相萃取净化后,采用液相色谱分离。以Poroshell 120EC-C18色谱柱为固定相,以不同体积比的甲醇和水的混合液为流动相进行梯度洗脱。质谱分析中采用多反应监测模式,外标法定量。灭多威和杀线威的质量浓度在5.00~200μg·L^(-1)内与其峰面积呈线性关系,检出限(3S/N)分别为3.0,0.2μg·kg^(-1)。按标准加入法在3个浓度水平上进行回收试验,回收率在66.5%~94.0%之间,测定值的相对标准偏差(n=6)在7.4%~11%之间。The sample （5. 000 0 g） was mixed with 10 mL of acetonitrile and 5 g of anhydrous sodium sulfate, and the solution was extracted by vertical oscillation for 30 min. The extract （2 mL） was purified with 14 mg of grapheme by dispersive solid phase extraction （DSPE）. The purified solution was then separated by LC using Poroshell 120 EC-C18 column as stationary phase and a mixture of methanol and water in various ratios as mobile phase in gradient elution. MRM was adopted in MS analysis, and external standard method was used for quantification. Linear relationships between values of peak area and mass concentration of methomyl and oxamyl were found in the range of 5.00--200 μg · L^-1 , with detection limits （3S/N） of 3. 0, 0. 2μg · L^-1, respectively. Test for recovery was made by standard addition at 3 concentration levels, giving results in the range of 66.5%-- 94. 0%, with RSDs （n=6） ranged from 7.4% to 11%.

关 键 词：液相色谱-串联质谱法 分散固相萃取 石墨烯 灭多威 杀线威 洋葱 

分 类 号：O657.63[理学—分析化学]