摘要
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.
出处
《食品工业科技》
CAS
CSCD
北大核心
2017年第15期244-247,252,共5页
Science and Technology of Food Industry
基金
山东省重点研发计划项目(2015GSF120018)
关键词
三聚氰胺
舒巴坦
亲水作用色谱-串联质谱法
原料乳
液体乳
melamine
sulbaetam
hydrophilie interaction chromatography tandem mass spectrometry ( HILIC- MS/MS )
raw milk
liquid milk