Gao Jie, Liu Qing, Han Feng, Miao Hong, Zhao Yunfeng, Wu Yongning
Wei Sheng Yan Jiu. 2014 May;43(3):449-54.
To establish a method for the determination of fatty acid esters of 3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD) in diet samples by gas chromatography-mass spectrometry (GC-MS) with solid-supported liquid-liquid extraction (SLE).
Diet samples were ultrasonically extracted by hexane, followed by ester cleavage reaction with sodium methylate in methanol, and then purified by solid-supported liquid-liquid extraction. (SLE) using diatomaceous earth as the sorbent. After derivatization with heptafluorobutyrylimidazole, the analytes were detected by GC-MS and quantified by the deuterated internal standards.
The limits of detection (LODs) of 3-MCPD esters and 2-MCPD esters in different diet samples were 0.002 - 0.005 mg/kg and 0.002 - 0.006 mg/kg. The average recoveries of 3-MCPD esters and 2-MCPD esters at the spiking levels of 0.05 and 0.1 mg/kg in the diet samples were in the range of 65.9% - 104.2% and 75.4% - 118.0%, respectively, with the relative standard deviations in the range of 2.2% - 14.2% and 0.8% - .13.9%.
The method is simple, accurate and rugged for the determination of fatty acid esters of 3-MCPD and 2-MCPD in diet samples.
建立一种采用固相支持液液萃取（SLE）结合气相色谱-质谱联用（GC-MS）法测定食品样品中3-氯-1,2-丙二醇（3-MCPD）和2-氯-1,3-丙二醇（2-MCPD）脂肪酸酯的方法。
食品样品用正己烷超声提取，然后在甲醇中与甲醇钠进行酯裂解反应，接着用硅藻土作为吸附剂通过固相支持液液萃取（SLE）进行净化。用七氟丁酰咪唑衍生化后，通过GC-MS检测分析物并用氘代内标进行定量。
不同食品样品中3-MCPD酯和2-MCPD酯的检测限分别为0.002 - 0.005 mg/kg和0.002 - 0.006 mg/kg。食品样品中3-MCPD酯和2-MCPD酯在0.05和0.1 mg/kg加标水平下的平均回收率分别为65.9% - 104.2%和75.4% - 118.0%，相对标准偏差分别为2.2% - 14.2%和0.8% - 13.9%。
该方法用于测定食品样品中3-MCPD和2-MCPD脂肪酸酯简单、准确且耐用。
