液相色谱-串联质谱法测定牛奶中伏马菌素FB_1和FB_2及其水解代谢物  

Determination of Fumonisins B_1,B_2 and Their Hydrolysed Metabolites in Bovine Milk by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：钱鸣蓉[1] 吴俐勤[1] 章虎[1] 刘飞 李锐[1] 陈志民[1] 方丽珍[1] 

机构地区：[1]浙江省食品安全重点实验室,浙江省农业科学院农产品质量标准研究所,杭州310021 [2]赛默飞世尔科技(上海)有限公司色谱质谱部,上海201206

出　　处：《分析化学》2012年第5期757-761,共5页Chinese Journal of Analytical Chemistry

基　　金：浙江省分析测试基金(No.2007F70026);2010年浙江省“三农五方”科技协作计划资助项目

摘　　要：建立了MAX混合阴离子固相萃取柱净化-高效液相色谱-串联质谱法测定牛奶中伏马菌素FB1和FB2及其水解代谢产物HFB1和HFB2的方法。牛奶样品经水稀释后,经MAX柱直接净化,甲醇洗脱得到FB1和FB2,经液相色谱-串联质谱负离子扫描测定,1%乙酸甲醇洗脱得到HFB1和HFB2,经液相色谱-串联质谱正离子扫描测定。结果表明,添加浓度为0.l～5.0μg/L,牛奶中FB1和FB2及其水解代谢产物的回收率为76.4%～92.3%;相对标准偏差(RSD,n=5)为5.9%～12.5%;方法检出限(LOD)均为0.03μg/L;定量限(LOQ)均为0.1μg/L。本方法操作简单,灵敏度、回收率和重复性均良好。MAX column combined with high performance liquid chromatography-tandem mass spectrometry was used to determine fumonisins B1（FB1）,FB2 and their hydrolysed metabolites in bovine milk.After 10 mL milk was diluted with 10 mL water,it was directly transferred to MAX column for purification.FB1 and FB2 were eluted with methanol and detected with HPLC-MS/MS in negative mode.The hydrolysed metabolites hydrolysed fumonisins B1（HFB1） and HFB2 were eluted with methanol containing 1% acetic acid and detected with HPLC-MS/MS in positive mode.The recoveries for four compounds were 76.4%-92.3% at fortification levels of 0.1-5 μg/L in bovine milk and relative standard deviation was in the range of 5.9%-12.5%.The LOD was 0.03 μg/L and LOQ was 0.1 μg/L for FB1,FB2 and their hydrolysed metabolites.This method is simple,sensitive,and repeatabilities with satisfied recoveries.

关 键 词：牛奶 伏马菌素 水解代谢产物 固相萃取 液相色谱-串联质谱 

分 类 号：R155.5[医药卫生—营养与食品卫生学]