氘代同位素内标GC/MS法测定食品中3-氯-1,2-丙二醇的方法研究

目的:建立以氘代同位素内标测定食品中3-氯-1, 2 -丙二醇的GC/MS方法。方法:试样中加入d5 -3 -氯-1, 2-丙二醇氘代同位素内标,用盐溶液提取试样中的3-MCPD,采用Extrelut硅藻土进行柱层析净化试样,经七氟丁酰基咪唑衍生化后, 用毛细柱气相色谱分离,采用选择离子监测(SIM)的质谱扫描模式进行定量分析。结果: 3-氯-1,2-丙二醇检测限低于0. 01mg/kg; 各类食品样品加标0. 01mg/kg的平均回收率>85%,样品重复测定6次的CV值均小于10%。结论:该方法具有较高的灵敏度、准确度、精密度和特异性,可满足欧盟和我国法规对痕量氯丙醇检测分析的要求,适用于可能含有3-MCPD的几乎所有食品。

Determination of 3-chloropropane-1,2-diol in food by using GC/MS

Objective:To develop a GC/MS method for the determination of 3-chloropropane-1,2-diol (3-MCPD) in food using deuterated internal standard.Methods:Samples were homogenized, mixed with salt solution after addition of internal standard d_5-3-MCPD and then adsorbed on Extrelut refill pack. The mixture was packed into a glass chromatographic column, from which 3-MCPD was extracted by elution with diethyl ether. Heptafluorobutyrylimidazole(HFBI) was added to the concentrated eluant to derivatise the chloropropanols and the derivatised analytes were separated by gas chromatography, identified and quantified by mass spectrometry.Results:The rates of recovery of 3-MCPD from various foods samples spiked at 0.01 mg/kg were more than 85%. The detection limit was less than 0.01 mg/kg and the CV values were less than 1%.Conclusion:The method is sensitive and precise for routine determination of 3-MCPD in a wide range of food and meets the requirements of tolerance limits adopted by EC and China.