超高效液相色谱-串联质谱法测定猪肾中安普霉素的残留量

Determination of Apramycin Residue in Pig Kidney by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了猪肾中安普霉素残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。猪肾样品以磷酸二氢钾溶液提取,经HLB固相萃取柱净化后,采用CAPCELL PAK MGⅡC_(18)(2.0 mm×150 mm,5μm)色谱柱分离,以0.1%甲酸水溶液和甲醇为流动相进行梯度洗脱。采用电喷雾离子源正离子模式扫描,多反应监测(MRM)模式进行检测,基质匹配同位素内标法定量。安普霉素在20~200μg/L质量浓度范围内线性良好,相关系数(r^(2))为0.9993,方法定量下限为10.0μg/kg。在10、20、100μg/kg加标水平下的平均回收率为85.5%~94.6%,相对标准偏差(RSD)不大于5.9%。该方法基于HLB固相萃取柱净化,基质匹配同位素内标法定量,具有操作简单、定性准确、灵敏度高的特点,适用于猪肾中安普霉素残留量的测定。

An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of apramycin residue in pig kidney was established.The pig kidney samples were extracted with KH2PO4 solution and purified by HLB solid phase extraction.The separation was performed by CAPCELL PAK MGⅡC_(18)(2.0 mm×150 mm,5μm)column by gradient elution,with 0.1%formic acid aqueous solution and methanol as mobile phases.The compound was analyzed in electrospray ion source positive ion mode under multi-reaction monitoring(MRM)mode.The matrix-matched isotope internal standard method was used for quantification.Apramycin showed good linearity in the concentration range of 20-200μg/L with a correlation coefficient(r^(2))of 0.9993.The limit of quantification was 10.0μg/kg.The average recoveries at spiked levels of 10,20,100μg/kg were 85.5%-94.6%with relative standard deviations(RSDs)not greater than 5.9%.Based on HLB solid phase extraction column purification and quantification by matrix-matched isotope internal standard method,this method has the characteristics of simple operation,accurate qualitative and high sensitivity.It is suitable for the determination of ampramycin residue in pig kidney.