固相萃取与气相色谱-质谱联用分析调味料中3-氯-1,2-丙二醇

建立固相萃取与气相色谱-质谱联用(solid phase extraction with gas chromatography-mass spectrometry，SPE-GC-MS)测定调味料中3-氯-1,2-丙二醇的新方法。对影响分析物SPE萃取效率的诸因素如洗脱溶剂、洗脱溶剂的体积和上样体积等进行详细考察和优化。最佳萃取条件为5.0g样品与5mol/L氯化钠溶液混匀，经SPE萃取净化、衍生后，以GC-MS进行测定，该方法对3-氯-1,2-丙二醇的检出限为0.15μg/kg，线性范围为0.51～6144μg/kg，相关系数和相对标准偏差(relative standard deviation，RSD)(n=5)分别为0.9998和8.8%。该方法成功应用于调味料3-氯-1,2-丙二醇的分析，加标回收的回收率为87.2%～109.4%。

Determination of 3-Monochloropropane-1,2-diol in Soy Sauce and Oyster Sauce by Solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry

A simple and sensitive method for determination of 3-monochloropropane-1,2-diol(3-MCPD) in sauce samples by solid phase extraction(SPE) coupled with with gas chromatography-mass spectrometry(GC-MS) is described.In this work,elution solvent type and amount and sample loading amount were investigated to optimize SPE conditions.The optimal sample preparation procedure for treating 5.0 g of samples involved homogenization with 5 mol/L sodium chloride solution,clean-up on SPE column and derivitization prior to G...