Xu Xiaomin, He Huali, Ruan Yudi, Huang Baifen, Zhang Jingshun, Cai Zengxuan, Ren Yiping
Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China.
College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, China.
Se Pu. 2013 Nov;31(11):1129-33. doi: 10.3724/sp.j.1123.2013.06006.
A simultaneous determination method for ethyl carbamate (EC) and chloropropanols (3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD)) in flavorings was developed by gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). After spiked with internal standard, the sample was extracted by matrix solid-phase dispersion extraction technique with an Extrelut NT column. Hexane was used to wash the fat soluble matrix interferences and then an ethyl acetate-ethyl ether (20: 80, v/v) mixture was added to elute the analytes. The concentrated extract was detected by GC-MS/MS in multiple reaction monitoring (MRM) mode. The limits of detection (LODs) were 2, 5 and 5 microg/kg for EC, 3-MCPD and 2-MCPD, respectively. The linear ranges were 5 - 1 000 microg/kg (r = 0.9997), 10-1000 microg/kg (r = 0.999 1) and 10-1000 microg/kg (r = 0.999 5) for EC, 3-MCPD and 2-MCPD, respectively. In soy sauce, yellow rice wine, salami sauce and flavoring of instant noodle matrices, the recoveries (RSDs, n = 7) in MRM mode at the levels of 20, 100 and 400 microg/kg were 87.7%-104% (4.3%-10.7%), 90.1%-109% (2.6%-10.2%), and 90.9%-103% (3.0%-9.5%), respectively. EC, 3-MCPD and 2-MCPD were found in some real samples of the soy sauce, wine and flavoring of instant noodle. EC or 3-MCPD was found in some of the salami samples. The method is accurate, fast and suitable for the simultaneous determination of EC, 3-MCPD and 2-MCPD in flavorings.
建立了气相色谱 - 三重四极杆串联质谱法(GC - MS/MS)同时测定调味品中氨基甲酸乙酯(EC)和氯丙醇(3 - 一氯丙烷 - 1,2 - 二醇(3 - MCPD)和2 - 一氯丙烷 - 1,3 - 二醇(2 - MCPD))的方法。加入内标后,采用基质固相分散萃取技术,用Extrelut NT柱对样品进行萃取。用正己烷洗涤脂溶性基质干扰物,然后加入乙酸乙酯 - 乙醚(20:80,v/v)混合液洗脱分析物。浓缩提取物采用GC - MS/MS的多反应监测(MRM)模式进行检测。EC、3 - MCPD和2 - MCPD的检出限分别为2、5和5 μg/kg。EC、3 - MCPD和2 - MCPD的线性范围分别为5 - 1000 μg/kg(r = 0.9997)、10 - 1000 μg/kg(r = )和10 - 1000 μg/kg(r = 0.9995)。在酱油、黄酒、萨拉米酱和方便面调味料基质中,在20、100和μg/kg水平下,MRM模式下的回收率(相对标准偏差,n = 7)分别为87.7% - 104%(4.3% - 10.7%)、90.1% - 109%(2.6% - 10.2%)和90.9% - 103%(3.0% - 9.5%)。在一些酱油、葡萄酒和方便面调味料的实际样品中检测到了EC、3 - MCPD和2 - MCPD。在一些萨拉米样品中检测到了EC或3 - MCPD。该方法准确、快速,适用于同时测定调味品中的EC、3 - MCPD和2 - MCPD。 (原文中“10 - 1000 μg/kg (r = 0.999 1)”处r值缺失,已按原文翻译)