在线凝胶渗透色谱-气质联用测定烟熏肉中7种N-亚硝胺类化合物的一测多评研究  

QAMS of seven N-nitrosamines compounds in smoked meat by online gel permeation chromatography-gas chromatography-mass spectrometry

作　　者：吕谦 尹明月 LÜQian;YIN Mingyue(Luzhou Market Inspection Testing Center,Luzhou 646000;College of New Energy Materials and Chemistry,Leshan Normal University,Leshan 614000)

机构地区：[1]泸州市市场检验检测中心,泸州646000 [2]乐山师范学院新能源材料与化学学院,乐山614000

出　　处：《中国食品添加剂》2025年第1期18-24,共7页China Food Additives

基　　金：四川省药品监督管理局科技计划项目(编号:2021007)。

摘　　要：为了建立基于一测多评的QuEChERS法结合在线凝胶渗透色谱技术检测烟熏肉中7种N-亚硝胺类化合物,烟熏肉样品在碱性环境中经乙腈提取,无水硫酸镁和无水乙酸钠去水,经C18、PSA净化,在线凝胶渗透色谱技术二次净化后,使用气质联用法进行检测。结果显示采用优化后的QuEChERS法结合在线凝胶渗透色谱,进一步消除了烟熏肉样品中的杂质,降低了基质效应。校正因子分别为ƒ_(NDMA/NPYR)=1.4073、ƒ_(NMEA/NPYR)=0.9491、ƒ_(NDEA/NPYR)=0.9433、ƒ_(NDPA/NPYR)=0.3822、ƒ_(NDBA/NPYR)=1.6247、ƒ_(NPIP/NPYR)=1.0263。7种N-亚硝胺类化合物检出限为0.03~0.25μg/kg;加标回收率及精密度分别为NDMA 103.4%~106.7%、2.4%~3.8%;NMEA 102.5%~107.6%、2.6%~3.8%;NDEA 102.7%~108.1%、2.5%~3.8%;NDPA 104.3%~106.4%、1.8%~3.9%;NDBA102.4%~108.3%、1.8%~3.7%;NPIP102.8%~106.8%、2.2%~3.6%;NPYR 102.5%~107.8%、2.1%~3.7%。该方法具有准确性好、过程简便等特点,可同时对大批量烟熏肉中7种N-亚硝胺类化合物快速测定。In order to establish a quantitative analysis of multi-components by single marker(QAMS)method for the determination of seven N-nitrosamines in smoked meat using QuEChERS combined with online gel permeation chromatography(GPC)technology.Smoked meat samples were extracted with acetonitrile under an alkaline condition,and dehydrated with anhydrous magnesium sulfate and anhydrous sodium acetate.After purification using C18 and PSA,the samples underwent further purification through online gel permeation chromatography,followed by detection using mass spectrometry.Results indicated that the optimized QuEChERS method combined with online GPC effectively removed impurities from smoked meat samples,reducing matrix effects.The correction factors were as follows:ƒ_(NDMA/NPYR)=1.4073,ƒ_(NMEA/NPYR)=0.9491,ƒ_(NDEA/NPYR)=0.9433,ƒ_(NDPA/NPYR)=0.3822,ƒ_(NDBA/NPYR)=1.6247,ƒ_(NPIP/NPYR)=1.0263.The detection limits for the seven N-nitrosamine compounds ranged from 0.03 to 0.25μg/kg.The recovery rates and precision for spiked samples were:NDMA 103.4%~106.7%(RSD 2.4%~3.8%);NMEA 102.5%~107.6%(RSD 2.6%~3.8%);NDEA 102.7%~108.1%(RSD 2.5%~3.8%);NDPA 104.3%~106.4%(RSD 1.8%~3.9%);NDBA 102.4%~108.3%(RSD 1.8%~3.7%);NPIP 102.8%-106.8%(RSD 2.2%~3.6%);NPYR 102.5%~107.8%(RSD 2.1%~3.7%).This accurate and efficient method facilitated the rapid and simultaneous determination of seven N-nitrosamines compounds in large batches of smoked meat products.

关 键 词：一测多评 N-亚硝胺类化合物 在线凝胶渗透色谱 气质联用 QUECHERS 

分 类 号：TS207.3[轻工技术与工程—食品科学]