GC-MS法快速检测酱油中的3-氯-1,2-丙二醇

Rapid determination of 3-monochloropropane-1,2-diol in soy sauce by using gas chromatography-mass spectrometry

目的:建立一种快速测定酱油中3-氯-1,2-丙二醇(3-MCPD)的GC-MS方法。方法:在试样中加入同位素内标(d5-3-MCPD),用正己烷净化,乙醚直接提取,经三乙胺催化的七氟丁酸酐(HFBA-Et3N)衍生,全扫描定性,选择离子定量。结果:方法的检出限为0.005 mg/kg,2种浓度水平下加标重复测定6次,相对标准偏差均小于10%,回收率为96.0%、104.0%,3-MCPD的进样量在0.010 ng～0.600 ng范围内线性良好(r=0.9993)。结论:该方法准确可靠、简单快速、经济环保,适用于酱油中3-MCPD的检测。

Objective：To establish a method for rapid determination of 3-monochloropropane-1,2-diol（3-MCPD） in soy sauce by gas chromatograph-mass spectrometry（GC-MS）.Methods：D5-3-MCPD was used as the deuterium isotope internal standard.The samples were cleaned up with n-hexane,then extracted by ethyl ether.The target compound was derivatized by heptafluor-oheptabutyric acid anhydride amended with triethylamine（HFBA-Et3N） and determination was performed by gas chromatograph-mass spectrometry at selective ions monitoring（SIM） mode.Results：The detection limit was 0.005 mg/kg,the recoveries were 96.0% and 104.0%（n=6） for the soy sauces spiked at two different levels,RSD〈10%,and a good linear relationship（r=0.9993） was obtained over the concentration range of 0.010 ng～0.600 ng.Conclusion：This method is accurate,rapid,economical,environmentally beneficial and suitable for routine determination of 3-MCPD in soy sauce.