论文部分内容阅读
目的建立一种Qu ECHERS-高效液相色谱-串联质谱法(HPLC-MS/MS),测定草莓中伊维菌素的残留。方法样品经含1%乙酸的乙腈溶液提取,Qu ECHERS方法净化后,以Phenomenex XB-C18(100 mm×2.1 mm,2.6μm)为分析色谱柱,甲醇和5 mmol/L乙酸铵-0.1%乙酸缓冲溶液为流动相进行梯度洗脱,采用MRM模式测定,外标法定量。结果样品经Qu ECHERS净化后,基质效应小,伊维菌素质量浓度为0.01 mg/L~2.0 mg/L时,线性关系良好,r=0.999 9,最低检出限为0.000 3 mg/kg,定量限为0.001 mg/kg。草莓中3种添加水平(0.02 mg/kg、0.10 mg/kg、1.00 mg/kg)的回收率为73.6%~105.5%,相对标准偏差(RSD)为1.2%~5.8%。结论将该法用于实际样品检测,结果表明,该方法操作简单,提取效果好,具有良好的灵敏度、回收率和重复性,适用于草莓中伊维菌素残留的分析测定。
Objective To establish a Qu ECHERS-HPLC-MS / MS method to determine the residues of ivermectin in strawberry. Methods The samples were extracted with 1% acetic acid in acetonitrile and purified by Qu ECHERS method. Phenomenex XB-C18 (100 mm × 2.1 mm, 2.6 μm) was used as the analytical column. Methanol and 5 mmol / L ammonium acetate- Buffer solution as the mobile phase gradient elution, using MRM mode determination, external standard method. Results When Qu ECHERS was used to purify the sample, the matrix effect was small. When the concentration of ivermectin was between 0.01 mg / L and 2.0 mg / L, the linearity was good, r = 0.999 9, the lowest detection limit was 0.000 3 mg / kg, The limit of quantification is 0.001 mg / kg. The recoveries of three kinds of strawberry (0.02 mg / kg, 0.10 mg / kg, 1.00 mg / kg) were 73.6% -105.5% with relative standard deviations (RSDs) of 1.2-5.8%. Conclusion The method is applied to the real sample testing. The results show that the method is simple, has good extraction efficiency, good sensitivity, recovery and repeatability. It is suitable for the determination of ivermectin residues in strawberry.