气相色谱-三重四极杆串联质谱法测定发酵食品中5种N-亚硝胺类化合物  

Determination of 5 N-Nitrosamine Compounds in Fermented Foods by Gas Chromatography-Triple Quadrupole Tandem Mass Spectrometry

作　　者：马嘉俊 傅春辉 杨瑞 平恬敏 傅华靖 刘镇 MA Jiajun;FU Chunhui;YANG Rui;PING Tianmin;FU Huajing;LIU Zhen(Shaoxing Testing Institute of Food and Drug,Shaoxing 312000,China)

机构地区：[1]绍兴市食品药品检验研究院,浙江绍兴312000

出　　处：《食品安全导刊》2025年第1期103-108,共6页China Food Safety Magazine

基　　金：绍兴市科技局产业关键技术攻关计划(2022B43003);浙江省省地协同项目(2024SDXT001-7)。

摘　　要：目的:建立气相色谱-三重四极杆串联质谱测定发酵食品中5种N-亚硝胺类化合物的分析方法。方法:样品经椰壳活性炭固相萃取小柱净化富集,采用大体积程序升温进样,经DB-1701色谱柱分离,采用多反应监测模式进行测定,以质量数和保留时间定性,内标法定量。结果:5种N-亚硝胺类化合物的浓度在25~1000μg·L^(-1)线性关系良好,相关系数均大于0.9960;方法检出限在0.1~0.8μg·kg^(-1),定量限在0.3~2.8μg·kg^(-1);样品的加标回收率为76.2%~112.1%,相对标准偏差在2.1%~8.1%。结论:该方法准确、可靠,适用于发酵食品酱油、黄酒中5种N-亚硝胺类化合物的检测。Objective:To establish a method for the determination of 5 N-nitrosamines in fermented food by gas chromatography-triple quadrupole tandem mass spectrometry.Method:The samples were purified and concentrated by a small column of solid phase extraction of coconut shell activated carbon,injected with a large volume temperature program,separated by DB-1701 chromatographic column,determined by multiple reaction monitoring mode,qualitative by mass number and retention time,quantitative by internal standard method.Result:The concentration of 5 N-nitrosamines was in the range of 25μg·L^(-1)to 1000μg·L^(-1),and the correlation coefficient was greater than 0.9960.The limits of detection and quantitation were 0.1μg·kg^(-1)to 0.8μg·kg^(-1)and 0.3μg·kg^(-1)to 2.8μg·kg^(-1).The recoveries ranged from 76.2%to 112.1%,and the relative standard deviation was 2.1%to 8.1%.Conclusion:The method is accurate and reliable,and is suitable for the determination of 5 N-nitrosamines in fermented food soy sauce and rice wine.

关 键 词：N-亚硝胺 发酵食品 气相色谱-三重四极杆串联质谱法 

分 类 号：TS207.3[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]