纷散固相萃取—超高效液相色谱—串联质谱法测定水产品中利福平残留

建立一种测定水产品中利福平药物残留的超高效液相色谱—串联质谱检测方法。样品用乙腈—二氯甲烷(6∶4,体积比)提取剂提取,通过100 mg C18+100 mg PSA分散固相萃取净化,以3 mmol/L乙酸铵溶液(含0.05%甲酸)和乙腈为流动相进行梯度洗脱,采用电喷雾离子源正离子多反应监测模式测定,内标法定量分析。检测结果显示,利福平在1~20μg/kg质量浓度内呈良好的线性关系,相关系数r≥0.9986,方法检出限为0.3μg/kg,定量限为1.0μg/kg,对罗非鱼、凡纳滨对虾、中华鳖进行加标回收试验,回收率为90.17%~101.07%,相对标准偏差为3.11%~7.66%,该方法简单、快速、准确,适用于水产品中利福平残留的确证和定量分析,为监管利福平药物的违规使用提供便捷、有效的技术支持。

Detection of Rifampicin in Fishery Products by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid Phase Extraction

A method was established for the detection of rifampicin residues in fishery products by ultra performance liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction.The samples were extracted with acetonitrile-dichloromethane(6∶4,V/V),purified by a mixture of 100 mg C18 and 100 mg ethylenediamine-N-propylsilane(PSA),and then eluted with 3 mmol/L ammonium acetate solution(containing 0.05%formic acid).The electrospray ionization mass spectrometry was operated in the positive mode using multiple reaction monitoring(MRM),and the target compound was quantified by the internal standard method.The results showed that the calibration curve for rifampicin exhibited good linear relationship in the range of 1—20μg/kg with correlation coefficients(r)of more than 0.9986,with detection limit of 0.3μg/kg and the quantification limit of 1.0μg/kg.The average recoveries for Nile tilapia hybrid Oreochromis aureus×O.niloticus,Pacific white shrimp Litopenaeus vannamei and Chinese soft shelled turtle Trionyx sinensis were ranged from 90.17%—101.07%with relative standard deviations(RSDs)of 3.11%—7.66%.The method is suitable for the detection and confirmation of rifampicin in fishery products due to its simplicity,rapidity,and high accuracy,and provides convenient and effective technical support for the supervision of illegal use of rifampicin.