液相色谱-串联质谱法测定淡水产品中的微囊藻毒素  

The Determination of the Microcystins in Freshwater Products by HPLC-MS/MS

作　　者：吴振兴[1] 鲍蕾[1] 赵华梅[1] 静平[1] 甘南琴[2] 

机构地区：[1]山东出入境检验检疫局,山东青岛266000 [2]中国科学院水生生物研究所,湖北武汉430072

出　　处：《食品研究与开发》2013年第22期21-24,共4页Food Research and Development

基　　金：国家质检总局科技项目<微囊藻毒素标准物质研制;毒素降解及检测技术的系统研究>资助项目

摘　　要：利用液相色谱-串联质谱法测定淡水产品虾和鱼中的微囊藻毒素MC-LR和MC-RR。试样以80%甲醇水溶液提取,再以固相萃取技术对微囊藻毒素进行富集净化,最后以液相色谱-串联质谱法定性定量分析。采用电喷雾离子源,正离子方式下进行多反应监测(MRM)。该方法检测限为1μg/kg,线性范围为0.5μg/kg^10.0μg/kg,MC-LR回收率范围为69.2%~95.6%,MC-RR回收率范围为71.6%~93.1%,变异系数为3.2%~7.3%。该方法操作简便,灵敏度高,选择性好,可以满足淡水产品中微囊藻毒素检测的相关要求。Microcystins LR and RR in freshwater products were determined by high performance liquid chromatography-triple quadrupole mass spectrometer. The toxins were extracted by 80 % methanol aqueous solution, then enriched and purified by solid phase extraction column, determined by HPLC-MS/MS with electron spray ion source under multiple reaction monitoring mode. The method LOQ was 1 Ixg/kg, the linear determination range was 0.5 Ixg/kg-10.0 Ixg/kg, and the recovery range of MC-LR and MC-RR are 69.2 %- 95.6 % and 71.6 %-93.1% respectively, the coefficient of variation range was 3.2 %-7.3 %. The method is easy to operate, and has high sensitivity, good selectivity. The method can meet the detection requirements of microcystins in freshwater products.

关 键 词：液相色谱-串联质谱 淡水产品 微囊藻毒素 

分 类 号：O657.63[理学—分析化学]