液相色谱-串联质谱法检测水发产品中氨基脲  

Determination of Semicarbazide in Waterish Logged Food Products by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：白亚敏 陈世奇 唐韵熙 江生 兰玉坤 BAI Yamin;CHEN Shiqi;TANG Yunxi;JIANG Sheng;LAN Yukun(Chongqing Institute for Food and Drug Control,Chongqing 401121,China;Key Laboratory of State Market Regulation(Condiment Supervision Technology),Chongqing 401121,China)

机构地区：[1]重庆市食品药品检验检测研究院,重庆401121 [2]国家市场监管重点实验室(调味品监管技术),重庆401121

出　　处：《现代食品》2022年第14期194-197,共4页Modern Food

基　　金：国家市场监督管理总局科技计划项目(S2019MK463)。

摘　　要：目的:建立液相色谱-串联质谱测定水发产品中氨基脲的分析方法。方法:样品经水洗涤除杂后,利用1 mol·L^(-1)盐酸水解,邻硝基苯甲醛衍生反应,乙酸乙酯提取,正己烷净化,Waters-C_(18)色谱柱分离,经乙腈(含0.1%甲酸)-10 mmol·L^(-1)乙酸铵水溶液(含0.1%甲酸)梯度洗脱,电喷雾正离子(ESI^(+))扫描,内标法测定。结果:氨基脲衍生物在0.5~20.0μg·kg^(-1)呈良好的线性关系,r>0.999,水发产品中氨基脲检出限为0.15~0.18μg·kg^(-1),平均回收率为73.9%~88.0%,RSD为3.2%~8.6%。结论:该方法重现性好,灵敏度高,定量准确,可用于水发产品中氨基脲的测定。Objective:An analytical method for the determination of semicarbazide in waterish logged food products was established and validated based on liquid chromatography-tandem mass spectrometry.Method:Samples were washed with water,hydrolyzed with 1 mol·L^(-1) hydrochloric acid,and then derivatized by 2-nitrobenzaldehyde.After extracted by ethyl acetate,and purified by hexane,the samples were loaded into C_(18) column,and separated with acetonitrile(0.1%formic acid)-10 mmol·L^(-1) ammonium acetate aqueous solution(0.1%formic acid)as the mobile phase.The electrospray ionization in positive ion mode(ESI^(+))was operated,and the internal standard method was used in the detection.Result:There was a good linear relationship in the range of 0.5~20.0μg·kg^(-1) concentration,r>0.999.The detection limits were 0.15~0.18μg·kg^(-1),the average recovery was 73.9%~88.0%and the RSD was 3.2%~8.6%.Conclusion:The method is sensitive,high repeatability and is accurate in determination of semicarbazide in waterish logged food products.

关 键 词：液相色谱-串联质谱法 水发产品 氨基脲 

分 类 号：O657.63[理学—分析化学]