加速溶剂萃取结合液相色谱-串联质谱同步检测肉、蜂蜜及乳制品中的双稠吡咯啶生物碱残留量  

Simultaneous determination of pyrrolizidine alkaloids residues in meat,honey and milk by accelerated solvent extraction coupled with liquid chromatography-tandem mass spectrometry

作　　者：徐文泱 张继红 赵红清 向俊 王凯 XU Wenyang;ZHANG Jihong;ZHAO Hongqing;XIANG Jun;WANG Kai(Hunan Institute of Food Quality Supervision Inspection and Research,Hunan Provincial Key Laboratoiy of Food Safety Monitoring and Early Warning,Changsha 410017)

机构地区：[1]湖南省食品质量监督检验研究院,食品安全监测与预警湖南省重点实验室,长沙410017

出　　处：《分析试验室》2021年第11期1284-1288,共5页Chinese Journal of Analysis Laboratory

基　　金：湖南创新型省份建设专项社会发展领域重点研发项目(2019SK2121);湖南省科技创新平台与人才计划项目(2019TP1058)资助。

摘　　要：采用加速溶剂萃取、固相萃取柱净化蜂蜜、乳制品及肉中的5种双稠吡咯啶生物碱,建立液相色谱-串联质谱的同时测定方法。样品以乙腈提取,MCX小柱净化,采用Eclipse Plus C_(18)柱进行分离,0.1%甲酸和0.1%乙酸铵水溶液以及乙腈为流动相洗脱,电喷雾电离正离子模式扫描,多反应监测测定,外标法定量分析。标准溶液在1~100 ng/mL范围内呈线性关系,相关系数大于0.99,方法定量限为0.05和0.5μg/kg,平均回收率在83.6%~88.0%,相对标准偏差小于10%。该方法将为动物源性食品中双稠吡咯啶生物碱的检测提供技术依据。An accelerated solvent extraction and solid phase extraction( SPE) were used to purify five kinds of pyrrolidine alkaloids in honey,meat and dairy products. A high performance liquid chromatography-tandem mass spectrometry( HPLC-MS/MS) method was developed for the simultaneous determination of these alkaloids. The samples were extracted by acetonitrile,purified by MCX column,separated by Eclipse Plus C;column,and eluted by mobile phase composing of 0. 1% formic acid,0. 1% ammonium acetate aqueous solution and acetonitrile. It adopted electrospray ionization positive ion scanning mode as well as multi-reaction monitoring and quantitative analysis with external standard method. The linear range of the method was 1-100 ng/m L and the linear correlation coefficient was above 0. 99. The detection limits of the method were 0. 05 and 0. 5 μg/kg.The average recoveries were in the range of 83. 6%-88. 0%,and the relative standard deviations were less than10%. This method will provide a technical basis for the detection of pyrrolidine alkaloids in animal-derived foods and offer support for the relative monitoring.

关 键 词：双稠吡咯啶生物碱 加速溶剂萃取 液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]