液相色谱-串联质谱法测定水产加工品中的甜蜜素  

Termination of sodium cyclamate in aquatic products by liquid chromatography-tandem mass spectrometry

作　　者：于慧娟[1] 惠芸华[1] 顾润润[1] 孔聪[1] 田良良[1] 

机构地区：[1]中国水产科学研究院东海水产研究所,农业部水产品风险评估实验室(上海),上海200090

出　　处：《分析试验室》2016年第7期809-812,共4页Chinese Journal of Analysis Laboratory

基　　金：上海市农业委员会农产品质量安全追溯体系开发与应用项目(沪农科推字(2016)第1-4-1号)资助

摘　　要：建立了液相色谱-串联质谱法测定水产加工品中甜蜜素的测定方法。样品用水提取,正己烷净化后,以0.1%甲酸-甲醇为流动相,C18色谱柱分离,在负离子模式下用配有电喷雾离子源的液相色谱-串联质谱测定。甜蜜素含量1~200 ng/m L范围内,线性关系良好(r^2=0.9999);方法定量限5μg/kg(S/N≥10)。甜蜜素在5μg/kg和50μg/kg添加水平下,平均回收率为81.0%~88.4%,相对标准偏差为4.0%~6.4%。方法适合水产加工品中甜蜜素的测定。本文根据甜蜜素的性质,选取水为提取剂,并对净化方法进行了研究,通过正已烷液-液萃取和冷冻方式去除了提取液中的油类物质和水溶性蛋白,确保了分析结果的稳定性和准确性。该技术的建立为水产加工品中甜蜜素监管提供技术支撑。A method of liquid chromatography-tandem mass spectrometry was developed for the determination of sodium cyclamate in aquatic products. The samples were extracted by water and purified by hexane. After separation with C18 column using 0. 1% formic acid-methanol as mobile phase,the sample solutions were determined by LC-MS / MS in negative mode（ ESI-）. The linear ranges were 1 ～ 200 ng /m L for sodium cyclamate with the correlation coefficient of 0. 9999. The limit of quantitative was 5 μg / kg（ S / N≥10）. The spike recoveries were81. 0% ～ 98. 4% in 5 and 50 μg / kg with relative standard derivation of 4. 0% ～ 6. 4%. This method is effective,simple,and suitable for the determination sodium cyclamate in various kinds of aquatic products.

关 键 词：液相色谱-串联质谱 甜蜜素 水产加工品 

分 类 号：TS207.3[轻工技术与工程—食品科学]