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当前位置: 首页 > 文章 > 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(英文) 食品科学 2011,32 (14) 232-236
Position: Home > Articles > Determination of 3-Monochloropropane-1,2-diol in Soy Sauce and Oyster Sauce by Solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry FOOD SCIENCE 2011,32 (14) 232-236

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(英文)

作  者：
熊珺;龚亮;赖毅东
单  位：
广东省东莞市质量监督检测中心
关键词：
固相萃取;3-氯-1,2-丙二醇;气相色谱-质谱联用;调味液
摘  要：
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%。
译  名：
Determination of 3-Monochloropropane-1,2-diol in Soy Sauce and Oyster Sauce by Solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry
作  者：
XIONG Jun,GONG Liang,LAI Yi-dong(Guangdong Dongguan Quality Supervision and Testing Center,Dongguan 523808,China)
关键词：
solid phase extraction;3-monochloropropane-1,2-diol;gas chromatography-mass spectrometry(GC-MS);sauce samples
摘  要：
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 GC-MS analysis.The limit of detection of the method for 3-MCPD was 0.15μg/kg,and the linear range 0.51-6144μg/kg,with a correlation coefficient of 0.9998 and a relative standard deviation of 8.8%(RSD,n = 5).The method was applied to determine soy sauce and oyster sauce samples and spiked recoveries of 87.2%-109.4% with RSDs(n = 3) of 5.6%-10.2% were obtained.

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