改进的QuEChERS结合气相色谱-三重四极杆质谱法快速测定酸肉中10种挥发性N-亚硝胺类化合物

采用改进的QuEChERS方法进行提取和净化,建立了气相色谱-三重四极杆质谱(GC-MS/MS)快速测定酸肉样品中10种挥发性N-亚硝胺类化合物的检测方法。样品经乙腈提取和正己烷除脂后,采用十八烷基硅烷键合硅胶(C18)和N-丙基乙二胺(PSA)混合吸附剂净化,采用DB-WAX色谱柱(30 m×0.25 mm×0.25μm)分离,在选择反应监测(SRM)模式下进行测定,外标法定量。10种N-亚硝胺类化合物在1~100μg/L范围内线性关系良好,相关系数(r)均0.99。10种N-亚硝胺类化合物的加标回收率为79.8%~115.3%,相对标准偏差(RSD)为0.6%~22.9%(n=6);方法的检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.04~0.3μg/kg和0.1~1μg/kg。该法简便快速,灵敏有效,适用于酸肉中N-亚硝胺类化合物的快速筛查和测定。

Rapid determination of 10 volatile N-nitrosamines in sour meats by modified QuEChERS and gas chromatography- triple quadrupole mass spectrometry

A rapid gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) method with modified QuEChERS method was developed for the determination of 10 volatile N-nitrosamines in sour meats. The samples were extracted with acetonitrile and eliminated the fat with n-hexane. The extracts in acetonitrile layer were purified by octadecyl silane (C18) and primary secondary amine (PSA) sorbents. The N-nitrosamines were determined on a DB-WAX column (30 m×0.25 mm×0.25 μm) by GC-MS/MS in selected reaction monitoring (SRM) mode. The external standard method was used to quantify the N-nitrosamines. The correlation coefficients (r) of the standard calibration curves were greater than 0.99 in the range of 1-100 μg/L. The average recoveries ranged from 79.8% to 115.3% with the relative standard deviations (RSDs) from 0.6% to 22.9% (n=6). The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) were 0.04-0.3 μg/kg and 0.1-1 μg/kg, respectively. The developed method is simple, rapid, sensitive and efficient for the screening of the N-nitrosamines in sour meats.