摘要
目的建立低共熔溶剂(deep eutectic solvent,DES)-超高效液相色谱-大气压化学离子化-串联质谱法快速测定火腿肠中9种N-亚硝胺污染物的分析方法。方法样品经水稀释,微量DES分散萃取,50%甲醇水复溶,Agilent Infinitylab Poroshell 120 EC-C_(18)(2.1 mm×150 mm,2.7μm)色谱柱分离,大气压化学电离源电离,多反应监测模式检测,内标法定量分析。结果9种N-亚硝胺在5.0~60.0ng/mL范围内线性关系良好,线性相关系数(r)均大于0.999。方法检出限为0.1~0.3μg/kg,定量限为0.3~1.0μg/kg,回收率为72.1%~111.6%,相对标准偏差为0.9%~8.4%。结论低共熔溶剂对N-亚硝胺的萃取效果佳,可以解决传统操作步骤烦琐的问题。本方法有机试剂用量少、绿色环保,适用于火腿肠中9种N-亚硝胺的快速、精准检测。
Objective To establish a rapid method for determination of 9 kinds of N-nitrosamines in ham sausage by ultra performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry with deep euectic solvent(DES).Methods The samples were initially dissolved in water,then extracted using microscale DES,subsequently re-dissolved in 50%methanol-water before separation by Agilent Infinitylab Poroshell 120 EC-C_(18)(2.1 mm×150 mm,2.7μm)column,and atmospheric pressure chemical ionization source ionization-multiple reaction monitoring-positive ion mode detection.Internal standard method was used for quantitative analysis.Results The linear relationships of 9 kinds of N-nitrosamines of 5.0–60.0 ng/mL were good.The correlation coefficients(r)of the 9 kinds of N-nitrosamines above 0.999,the limits of detection were 0.1-0.3μg/kg,and the limits of quantification were 0.3-1.0μg/kg.The recovery rates were 72.1%-111.6%and relative standard deviations of 0.9%-8.4%.Conclusion DES has a good extraction effect of N-nitrosamines,which can solve the problem of complicated tradittional operation steps.The method is environmentally friendly and requires a small amount of organic reagents.It is suitable for the rapid and accurate detection of 9 N-nitrosamines in ham sausage.
作者
郑鸿涛
谢国丹
谭贵良
刘子雄
董海
柯坚灿
ZHENG Hong-Tao;XIE Guo-Dan;TAN Gui-Liang;LIU Zi-Xiong;DONG Hai;KE Jian-Can(Zhongshan Institute for Food and Drug Control,Zhongshan 528437,China;Zhongshan Institute,University of Electronic Science and Technology of China,Zhongshan 528402,China)
出处
《食品安全质量检测学报》
CAS
2024年第14期52-58,共7页
Journal of Food Safety and Quality
基金
广东省自然科学基金项目(2020A1515011308)
中山市社会公益与基础研究项目(2020B2033、2021B2061)。
关键词
低共熔溶剂
N-亚硝胺
绿色提取
超高效液相色谱-大气压化学离子化-串联质谱法
火腿肠
deep eutectic solvent
N-nitrosamines
green extraction
ultra performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry
ham sausage
作者简介
郑鸿涛,高级工程师,主要研究方向为食品安全检测与研究。E-mail:65130078@qq.com;通信作者:谭贵良,博士,教授,主要研究方向为食品质量与安全。E-mail:joe88tan@126.com。
