气相色谱-三重四极杆质谱联用法检测市售腊肠中9种挥发性亚硝胺

Determination of Nine Volatile Nitrosamines in Local Sausage on Sale by Gas Chromatography Tandem Triple Quadrupole Mass Spectrometry

采用QuEChERS方法对市售腊肠中的N-亚硝基二甲胺（NDMA）、N-亚硝基二乙胺（NDEA）、N-亚硝基甲乙胺（NMEA）、N-亚硝基二丙胺（NDPA）、N-亚硝基吡咯烷（NPYR）、N-亚硝基哌啶烷（NPIP）、N-亚硝基二丁胺（NDBA）、N-亚硝基吗啉（NMOR）、N-亚硝基二苯胺（NDPhA）9种对人体有致癌活性的挥发性亚硝胺进行分离净化,气相色谱-三重四极杆质谱联用法（GC-MS/MS）检测。最佳实验条件下,9种挥发性亚硝胺的线性范围为0.25~200μg/L,检出限为0.01~0.10μg/kg,加标回收率为90.7%~116.0%,相对标准偏差（RSD）为1.8%~14.0%。市售腊肠样品中NDMA,NMOR,NPYR,NDPA,NPIP,NDBA,NDPhA均有不同程度的检出,总挥发性亚硝胺的含量为1.85~13.44μg/kg。该方法灵敏度高、操作简单,适合批量样品的快速检测。

A selective gas chromatography tandem triple quadrupole mass spectrometry was used to detect nine volatile nitrosamines,including N-nitrosodimethylamine（ NDMA）,N-nitrosodiethylamine（ NDEA）,N-nitrosomethylethylamine（ NMEA）,N-nitrosodipropylamine（ NDPA）,N-nitrosopyrrolidine（ NPYR）, N-nitrosopiperidine（ NPIP）, N-nitrosodibutylamine（ NDBA）, N-nitrosomorpholine（ NMOR）,N-nitrosodiphenylamine（ NDPhA） in local sausage on sale by using QuEChERS sample pretreatment. The calibration curves of nine volatile nitrosamines were linear in the range of 0. 25-200 μg / L,with detection limits of 0. 01- 0. 10 μg / kg. The recoveries were in the range of 90. 7%-116. 0% at three spiked concentration levels in sample,with relative standard deviations（ RSDs） of1. 8%- 14. 0%. The method was applied in the detection of local sausage on sale,and seven volatile nitrosamines were all detected. The detection rates of NDMA, NMOR, NPYR, NDPA were higher than that of the others. The contents of total volatile nitrosamines were in the range of 1. 85-13. 44 μg / kg. The developed method was simple,rapid,sensitive and accurate.