高效液相色谱-高分辨质谱法快速测定猪肉中的阿托品和普鲁卡因残留

Rapid determination of atropine and procaine residues in pork by high performance liquid chromatography-high resolution mass spectrometry

目的建立高效液相色谱-高分辨质谱法测定猪肉中阿托品和普鲁卡因残留的分析方法。方法样品经乙腈提取,采用通过式吸附净化柱净化,高效液相色谱C_(18)柱分离化合物,高分辨质谱分析测定,平行反应监测模式定量检测,外标法定量。结果阿托品和普鲁卡因保留时间分别为5和4 min,在0.1~5.0μg/kg之间线性关系良好,批内、批间精密度均小于20%,回收率稳定在85%~105%之间,定量限为0.1μg/kg。结论该方法灵敏、快速、准确度高,可用于监测猪肉中2种药物残留,可为畜产品质量安全保障提供高效的技术支撑。

Objective To establish an analytical method for determination of atropine and procaine residues in pork by high performance liquid chromatography-high resolution mass spectrometry.Methods The samples were extracted with acetonitrile,purified by a mobile adsorption purification column,and the compounds were separated on a high performance liquid chromatography C 18 column,analyzed and determined by high-resolution mass spectrometry,detected quantitatively in parallel reaction monitoring mode,and quantified by external standard method.Results The retention times of atropine and procaine were 5 and 4 min,respectively.The linear relationships were good within the range of 0.1-5.0μg/kg.The intra-assay and inter-assay precision were less than 20%,the recoveries were stable within the range of 85%-105%,and the limits of quantification were 0.1μg/kg.Conclusion This method is sensitive,rapid and accurate,and can be used to monitor the residues of 2 kinds of drugs in pork,which can provide efficient technical support for the quality and safety assurance of livestock products.