气相色谱-串联质谱法测定肉制品中9种N-亚硝胺化合物

Determination of 9 N-Nitrosamine Compounds in Meat Products by Gas Chromatography-Tandem Mass Spectrometry

建立了QuEChERS结合气相色谱-串联质谱法同时测定肉制品中9种N-亚硝胺化合物的方法。样品经乙腈提取,用硫酸镁和氯化钠萃取,上清液用乙二胺-N-丙基硅烷(PSA)、硅胶键合十八烷基(HC-C18)和硫酸钠进行净化,离心后取上清液在优化好的仪器条件下进行测定;选用DB-WAX UI毛细管色谱柱,在程序升温条件下进行色谱分离,并在电子轰击源(EI)和选择离子监测模式(SIM)下进行质谱分析。结果显示,9种N-亚硝胺化合物在0~100μg/L范围内有良好的线性关系,检出限为0.07~0.30μg/kg,定量限为0.20~1.00μg/kg;选取香肠、肉松、酱肉3种空白基质样品,进行3个浓度水平的加标回收实验,测得的加标回收率为80.3%~110.2%,相对标准偏差(n=6)为1.3%~7.5%。此方法简单快速,适合高通量样品的分析测定。

A method was developed for the simultaneous determination of 9 N-nitrosamine compounds in meat products by QuEChERS combined with gas chromatography-tandem mass spectrometry.The samples were mixed with acetonitrile,then extracted with magnesium sulfate and sodium chloride.The supernatant was purified with ethylenediamine-N-propylsilane(PSA),silica-bonded octadecyl(HC-C18)and sodium sulfate,and measured under the optimized instrument conditions after centrifuging.Then,the N-nitrosamine compounds were separated under the programmed temperature conditions by using the DB-WAX UI capillary column.In the mass spectrometry analysis,electron impact source(EI)and selected ion monitoring mode(SIM)were adopted for the determination.The results showed that the 9 N-nitrosamine compounds had a good linear relationship in the range of 0~100μg/L.The detection limit was found between 0.07~0.30μg/kg and the quantification limit 0.20~1.00μg/kg.Sausage,pork floss and sauce pork were selected as blank matrix samples to subject to standard addition recovery tests at 3 concentration levels.The measured addition recovery rates ranged from 80.3%to 110.2%,and the relative standard deviation(n=6)was in the range of 1.3%~7.5%.This method was simple and fast,suitable for the analysis and determination of high-throughput samples.