Zhao Zhuang, Xu Yangbiao, Liu Xianghong, Shi Xiaoguang, Lu Yixiang
Guangxi Institute for Food and Drug Control, Nanning 530021, China.
Se Pu. 2017 Oct 8;35(10):1086-1093. doi: 10.3724/SP.J.1123.2017.06006.
A rapid gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) method with modified QuEChERS method was developed for the determination of 10 volatile -nitrosamines in sour meats. The samples were extracted with acetonitrile and eliminated the fat with -hexane. The extracts in acetonitrile layer were purified by octadecyl silane (C18) and primary secondary amine (PSA) sorbents. The -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 -nitrosamines. The correlation coefficients () 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% (=6). The limits of detection (LODs, =3) and limits of quantification (LOQs, =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 -nitrosamines in sour meats.
建立了一种采用改进的QuEChERS方法的快速气相色谱 - 三重四极杆质谱（GC-MS/MS）法，用于测定酸肉中的10种挥发性亚硝胺。样品用乙腈提取，并用正己烷去除脂肪。乙腈层提取物用十八烷基硅烷（C18）和伯仲胺（PSA）吸附剂净化。亚硝胺在DB-WAX柱（30 m×0.25 mm×0.25μm）上采用GC-MS/MS的选择反应监测（SRM）模式进行测定。采用外标法对亚硝胺进行定量。标准校准曲线在1 - 100μg/L范围内的相关系数（）大于0.99。平均回收率在79.8%至115.3%之间，相对标准偏差（RSD）为0.6%至22.9%（=6）。检测限（LOD，=3）和定量限（LOQ，=10）分别为0.04 - 0.3μg/kg和0.1 - 1μg/kg。所建立的方法对于酸肉中亚硝胺的筛查简单、快速、灵敏且高效。
