磁性固相萃取前处理-超高效液相色谱-串联质谱法测定牛奶中阿维菌素类药物残留

Determination of residues of avermectins in milk by magnetic solid phase extraction pre-treatment coupled with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  mSPE  LC-MS/MS  磁固相萃取  牛奶  阿维菌素

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  magnetic solid phase extraction  milk  avermectins

中文摘要:

      目的 建立磁性固相萃取(magnetic solid phase extraction, MSPE)前处理-超高效液相色谱-串联质谱法测定牛奶中阿维菌素类药物残留的方法。方法 牛奶样品使用乙酸锌和亚铁氰化钾沉淀蛋白, 8 mL乙腈提取, 10 mg磁性HLB净化材料净化, 5%乙腈-水、乙腈进行淋洗和洗脱, 使用超高效液相色谱-串联质谱法检测牛奶中阿维菌素、乙酰氨基阿维菌素、伊维菌素和多拉菌素。结果 4种药物在0.2~200.0 μg/L质量浓度范围内线性关系良好(r2>0.995)。阿维菌素、伊维菌素和多拉菌素的检出限为0.2 μg/kg, 定量限为0.5 μg/kg; 乙酰氨基阿维菌素的检出限为0.5 μg/kg, 定量限为2.5 μg/kg, 回收率为74.31%~96.67%, 相对标准偏差为0.02%~12.24%。结论 本研究建立的MSPE前处理技术, 极大地提高了样品前处理效率, 缩短了样品检测的时间, 降低了检测成本, 减少了有机溶剂的使用, 可应用于定量检测牛奶样品中阿维菌素类药物残留, 为MSPE前处理方法的广泛应用提供参考。

英文摘要:

      Objective To establish a method for the determination of avermectin residues in milk by magnetic solid phase extraction (MSPE) pre-treatment ultra performance liquid chromatography-tandem mass spectrometry. Methods Protein in milk samples was precipitated by zinc acetate and potassium ferrocyanide, samples were then extracted with 8 mL of acetonitrile, purified with 10 mg of magnetic HLB purification material, and washed and eluted with 5% acetonitrile-water and acetonitrile. Ultra performance liquid chromatography-tandem mass spectrometry was used to detect avermectin, eprinomectin, ivermectin and doramectin in milk. Results The linear relationship of the 4 kinds of drugs was good in the mass concentration range of 0.2?200.0 μg/L (r2>0.995). The limit of detection and limit of quantitation of abamectin, ivermectin and dolamectin were 0.2 μg/kg and 0.5 μg/kg, respectively. The limit of detection and limit of quantitation of acetylamictin were 0.5 μg/kg and 2.5 μg/kg, respectively. The recoveries were 74.31%–96.67% and the relative standard deviations were 0.02%–12.24%. Conclusion The MSPE pretreatment technology established in this paper greatly improves the sample pretreatment efficiency, shortens the sample detection time, reduces the detection cost, and reduces the use of organic solvents. It can be applied to the quantitative detection of abamectin drug residues in milk samples, and provides a reference for the wide application of MSPE pretreatment method.