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,CycDs)含量的方法。实验表明,3-MPD和CycDs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CycDs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%,CycDs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 (CycDs). The results demonstrated that the concentration of 3-MPD and CycDs 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 CycDs 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 CycDs. The intra- and inter- day precisions were 2.05% and 4.14% for 3-MPD, 1.18% and 2.82% for CycDs. 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.
[1] DING Wentao, ZHANG Guochang, LIU Jingjing. 3′ Truncation of the GPD1 promoter in Saccharomyces cerevisiae for improved ethanol yield and productivity[J]. Applied & Environmental Microbiology, 2013, 79(10): 3 273-3 281.
[2] DENADAL E, ALEPUZ P M, POSAS F. Dealing with osmostress through MAP kinase activation[J]. Embo Reports, 2002, 3(8): 735-740.
[3] 郭在力. 菌种及理化条件对冰葡萄酒发酵的影响[D].大连: 大连工业大学, 2016.
[4] GONG Xue, JIANG Lu, LIU Ning, et al. Screening and evaluation of yeast strains for producing wine higher in glycerol and lower in hydrogen sulphide[J]. Food Science, 2015, 36(19): 132-136.
[5] 尤雅, 段长青, 燕国梁. 扁平云假丝酵母与酿酒酵母混合发酵对葡萄酒乙醇含量及香气的影响[J]. 食品科学, 2018, 39(20): 157-165.
[6] 张烨, 孙玉梅, 俞志敏, 等. 糖分对葡萄酒发酵的影响[J]. 食品与发酵工业, 2017, 43(4): 285-290.
[7] BOVO B, NADAI C, VENDRAMINI C, et al. Aptitude of Saccharomyces yeasts to ferment unripe grapes harvested during cluster thinning for reducing alcohol content of wine[J]. International Journal of Food Microbiology, 2016, 236(7): 56-64.
[8] 原苗苗, 赵新节, 孙玉霞. 低温对葡萄酒香气成分和酵母代谢的影响[J]. 食品与发酵工业, 2017, 43(12): 268-276.
[9] ALE C E, BRU E, DE SAAD A M S, et al. Effect of physicochemical factors on glycerol production by simultaneous cultures of wine micro‐organisms using the response surface method[J]. Journal of Applied Microbiology, 2015, 117(5): 1 336-1 347.
[10] FAUHL C, WITTKOWSKI R, LOFTHOUSE J, et al. Gas chromatographic/mass spectrometric determination of 3-methoxy-1,2-propanediol and cyclic diglycerols, by-products of technical glycerol, in wine: Interlaboratory study[J]. Journal of Aoac International, 2004, 87(5): 1 179-1 188.
[11] COMITINI F, GOBBI M, DOMIZIO P, et al. Selected non-Saccharomyces wine yeasts in controlled multistarter fermentations with Saccharomyces cerevisiae[J]. Food Microbiology, 2011, 28(5): 873-882.
[12] 朱济义, 杜金华, 王秀菊, 等. 葡萄酒中甘油的生成及其影响因素[J]. 酿酒, 2010, 37(2): 23-27.
[13] ZHAO Xiangdong, PROCOPIO S, BECKER T. Flavor impacts of glycerol in the processing of yeast fermented beverages: A review[J]. Journal of Food Science & Technology, 2015, 52(12): 7 588-7 598.
[14] GAWEL R, SLUYTER S V, WATERS E J. The effects of ethanol and glycerol on the body and other sensory characteristics of Riesling wines[J]. Australian Journal of Grape & Wine Research, 2010, 13(1): 38-45.
[15] 郝良敏, 郝良磊, 李晓霞, 等. 酿酒酵母对葡萄酒品质的影响[J]. 河南农业, 2018(27): 43;50.
[16] 李记明, 姜文广. 优质干红葡萄酒中主要质量指标的研究[J]. 中外葡萄与葡萄酒, 2018(6): 18-24.
[17] 刘苑琳, 李辉, 张衡, 等. 葡萄酒活性干酵母直投和活化工艺对酒精发酵的影响[J]. 中国酿造, 2019, 38(9): 102-106.
[18] 刘锐萍, 赵广西, 杨帛, 等. 葡萄酒中有机酸和甘油掺伪鉴别检测方法的研究[J]. 酿酒科技, 2018(1): 41-46.
[19] 陈景桦, 马小琛, 李婷, 等. 优选发酵毕赤酵母与酿酒酵母混合发酵的葡萄酒酿造应用潜力[J]. 食品科学技术学报, 2018, 36(5): 26-34.
[20] 谢诗怡, 韩月, 张烨, 等. 不同有机氮源对葡萄酒发酵的影响[J]. 中国酿造, 2018, 37(4): 38-43.
[21] 张丽萍, 李伟辉, 徐江华. 葡萄酒中乙醇和甘油含量分析方法研究[J]. 食品研究与开发, 2016, 37(1): 174-176.
[22] 赵贝贝, 刘慧燕, 方海田, 等. 基于途径分析的产甘油有孢汉逊酵母菌株的选育[J]. 中国酿造, 2018, 37(7): 132-137.
[23] 刘青, 刘朝霞, 李志勇, 等. 葡萄酒中甘油含量的测定及其在品质鉴别中的应用[J]. 酿酒科技, 2015(1): 77-81.
[24] 刘青, 刘朝霞, 李志勇, 等. 国产葡萄酒中甘油含量的调查与分析[J]. 中国食品卫生杂志, 2015, 27(2): 171-175.
[25] 岳红卫, 郑淼, 郭新光, 等. 葡萄酒真实性及鉴别方法研究[J]. 食品研究与开发, 2017, 38(3): 212-216.
