GC-MS法测定酱油及调味液中的氯丙醇

Determination of Chloropropanols in Soy sauce and Seasoning Liquid by Gas Chromatography/Mass Spectrometry

目的:建立酱油及调味液中氯丙醇的GC-MS测定方法。方法:采用3-氯-1,2-丙二醇(3-MCPD)的氘代同位素d5-3-氯-1,2-丙二醇(d5-3-MCPD)做内标,使用硅藻土萃取SPE小柱快速分离提取,提取物经七氟丁酰基咪唑衍生后,用选择离子监测的气相色谱-质谱联用法测定3-氯-1,2-丙二醇的含量。结果:3-MCPD在0.02～0.50mg/L范围内线性良好(r>0.999),三个浓度水平下加标回收率为78.1%～85.7%,精密度6.2%～8.4%。结论:方法快速简便且具有较高的灵敏度、准确度、精密度和特异性,满足了酱油及调味液中痕量氯丙醇的分析要求。

Objective： To establish GC-MS method for determination of chloropropanols in soy sauce and seasoning liquid. Methods： Using d5-3-MCPD as deuterated internal standard, extracted by Diat- omite Solid Phase Extraction Cartridges, derivatised with HFBI reagent and determined by GC-MS in SIM mode. Results： The method has a good linear and the detection limits range from 0. 02 0.50 mg/L（r〉0.999）. The recoveries are 78.1%-85.7%, the relative standard derivation is 6.2%-8.4%. Conclusion： The method has high sensitivity, precision, accuracy and specificity, and it can be applied to detect chloropropanols in soy sauce and seasoning liquid.