超高效液相色谱-串联质谱法测定乳及乳制品中苯菌酮的残留量

Determination of metrafenone residues in milk and milk products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  固相萃取  乳及乳制品  苯菌酮  农药残留

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  solid phase extraction  milk and dairy products  metrafenone  pesticide residue

中文摘要:

      目的 建立一种超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)对乳及乳制品中苯菌酮的残留量进行定量的检测方法。方法 样品经1%甲酸乙腈提取, 经Prime HLB固相萃取小柱净化, 以ACQUITY UPLC BEH Phenyl色谱柱(100 mm×2.1 mm, 1.7 μm)分离, 使用乙腈-0.1%甲酸水作为流动相进行梯度洗脱, 扫描方式在电喷雾离子源正离子模式下采用多反应监测(multiple reaction monitoring, MRM)模式, 采用基质匹配标准曲线校准, 外标法定量。结果 苯菌酮在1.0~200.0 μg/L范围内线性关系良好, 相关系数(r)均不小于0.9960。方法检出限及方法定量限分别为1.5 μg/kg与5.0 μg/kg。在3个添加水平的加标回收实验下, 苯菌酮的平均回收率为84.1%~107.5%, 相对标准偏差为1.0%~7.2% (n=6)。结论 本方法前处理操作简便、结果准确、灵敏度高, 适用于乳及乳制品中苯菌酮残留量的测定。

英文摘要:

      Objective To establish an analytical method for the quantitative determination of metrafenone residues in milk and milk products by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with 1% formic acid-acetonitrile and purified by Prime HLB solid-phase extraction column. The samples were separated on an ACQUITY UPLC BEH Phenyl column (100 mm×2.1 mm, 1.7 μm). Acetonitrile-0.1% formic acid-water was used as the mobile phase for gradient elution. The scanning mode was multiple reaction monitoring (MRM) in positive ion mode of electrospray ion source, and matrix matching standard curve was used for calibration and external standard for quantification. Results The linearity was good in the range of 1.0?200.0 μg/L and the correlation coefficients (r) were not less than 0.9960. The limits of detection and limits of quantitation were 1.5 and 5.0 μg/kg, respectively. Under the spiked recovery experiments at the 3 levels of addition, the average recoveries of metrafenone were 84.1%?107.5%, and the relative standard deviations were 1.0%?7.2% (n=6). Conclusion This method is simple, accurate and sensitive, and is suitable for the determination of metrafenone residues in milk and milk products.