亲水作用色谱-串联质谱同时测定原料乳和液体乳中三聚氰胺和舒巴坦

Determination of melamine and sulbactam in raw milk and liquid milk by hydrophilic interaction chromatography tandem mass spectrometry

建立了亲水作用色谱-串联质谱同时测定原料乳和液体乳中三聚氰胺和舒巴坦的分析方法。试样采用2%乙酸水溶液提取,经乙腈沉淀蛋白,以乙腈-乙酸铵溶液为流动相,经Acquity UPLC BEH HILIC色谱柱分离后,采用多反应监测(MRM)扫描,外标法定量。三聚氰胺定量下限为10μg/kg,加标回收率为85.4%~102.5%,相对标准偏差为3.10%~6.55%。舒巴坦检定量下限为1.0μg/kg,加标回收率为86.1%~104.3%,相对标准偏差为2.35%~5.37%。该方法前处理简便快捷,灵敏度高,回收率和重现性良好,适用于原料乳和液体乳中三聚氰胺和舒巴坦的测定。

An analytical method was developed for the determination of melamine and sulbactam in raw milk and liquid milk using hydrophilic interaction chromatography tandem mass spectrometry（ HILIC-MS/MS）.The samples were extracted with 2%0 acetic acid solution,and the protein was precipitated with acetonitrile subsequently.The separations of melamine and sulbactam were carried out on an Aequity UPLC BEH HILIC column using ammonium acetate solution-acetonitrile as mobile phase.The target compounds were carried out in the multiple reaction monitoring （MRM）mode by employing the extelxlal standard method.The quantitation limit of mlamine wasl0 μg/kg.The recovery of melamine was 85.4%-102.5% ,with the RSD of 3.10% ~6.55% .The quantitation limit of sulbaetam was 1.0 txg/kg.The recovery of sulbactam was 86.1%0-104.3% , with the RSD of 2.35%-5.37%.With the advantages of convenience, sensitivity, good recoveries and repeatability,the method was suitable for the detection of melamine and sulbactam in raw milk and liquid milk.