气相色谱-质谱法检测葡萄酒中外源工业甘油副产物  

Determination of exogenous technical glycerol by-products in wine by gas chromatography-mass spectrometry (GC-MS)

作　　者：王广浩 高红波 樊双喜 李国辉 钟其顶 李艳[1] WANG Guanghao;GAO Hongbo;FAN Shuangxi;LI Guohui;ZHONG Qiding;LI Yan(College of Bioscience and Bioengineering,Hebei University of Science and Technology,Shijiazhuang 050018,China;China National Institute of Food and Fermentation Industries Co.,Ltd.,Beijing 100015,China;National Standardization Center of Food and Fermentation Industry,Beijing 100015,China)

机构地区：[1]河北科技大学生物科学与工程学院,河北石家庄050018 [2]中国食品发酵工业研究院有限公司,北京100015 [3]全国食品发酵标准化中心,北京100015

出　　处：《食品与发酵工业》2020年第16期215-219,共5页Food and Fermentation Industries

基　　金：科技部国家重点研发计划(2016YFE0113200,2017YFE0110800);科技部“十三五”重大科技计划(2016YFF0203903);国家自然科学基金(31601553,31601580);欧盟地平线2020计划(635690-OLEUM,727864-EU-China-Safe)。

摘　　要：该文验证了一种气相色谱-质谱法测定葡萄酒中外源工业甘油副产物3-甲氧基-1,2-丙二醇(3-methoxypropane-1,2-diol,3-MPD)和环二甘油(cyclic diglycerols,Cyc Ds)含量的方法。实验表明,3-MPD和Cyc Ds分别在0.10-2.00 mg/L和0.50-4.00 mg/L线性关系良好,R2均> 0.999;3-MPD和Cyc Ds的加标回收率分别为97.50%-101.11%和100.33%-104.67%,检出限分别0.02 mg/L和0.08 mg/L;3-MPD日内精密度与日间精密度分别为2.05%与4.14%,Cyc Ds日内精密度与日间精密度分别为1.18%与2.82%;对比样品的测定结果与德国联邦风险评估研究所(Bundesinstitut für Risikobewertung,BfR)相比,无显著性差异(P> 0.05)。该文首次在国内对葡萄酒中外源工业甘油副产物含量进行了检测,弥补了国内葡萄酒中外源工业甘油检测方法的缺失,为葡萄酒中外源工业甘油副产物的限量标准制定及掺假分析提供了方法支持。A gas chromatography-mass spectrometry (GC-MS) method was verified for the determination of exogenous technical glycerol by-products,3-methoxypropane-1,2-diol (3-MPD) and cyclic diglycerols (Cyc Ds). The results demonstrated that the concentration of 3-MPD and Cyc Ds had good linearity in the range of 0. 10-2. 00 mg/L and 0. 50-4. 00 mg/L,respectively,with R2 greater than 0. 999. The recoveries of 3-MPD and Cyc Ds were 97. 50%-101. 11% and 100. 33%-104. 67%,respectively. The limits of detection were 0. 02 mg/L for 3-MPD and 0. 08 mg/L for Cyc Ds. The intra-and inter-day precisions were2. 05% and 4. 14% for 3-MPD,1. 18% and 2. 82% for Cyc Ds. There was no significant difference in results of comparison samples from the Bundesinstitut für Risikobewertung (BfR) (P > 0. 05). This is the first time to detect the contents of exogenous technical glycerol by-products in wines in China,which introduces a new way to identify the authenticity of wine glycerol for China and provides method for the limited standards and adulteration analysis of exogenous technical glycerol by-products in wine.

关 键 词：气相色谱-质谱法 葡萄酒 外源工业甘油 真实性 掺假 

分 类 号：TS262.6[轻工技术与工程—发酵工程] O657.63[轻工技术与工程—食品科学与工程]