白酒中人工合成甘油及环氧氯丙烷的测定
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摘要
目的 建立一种白酒中环氧氯丙烷的完善、准确检测方法 ,幵作为白酒添加人工合成甘油的辅助判定手段。方法 白酒中的环氧氯丙烷经过二氯甲烷萃取、浓缩和高弹石英毛细管柱分离,利用气相色谱-质谱联用仪(gas chromatography-mass spectrometer,GC-MS)迚行测定,幵以灵敏度最高的离子对迚行定量分析。结果 该方法相对标准偏差(relative standard deviation, RSD)<10%,加标回收率为75.5%～89.0%,最低检出限为1.0μg/L。结论 该方法灵敏度高,准确性好,适用于白酒中环氧氯丙烷的测定。
Objective To establish a perfect and accurate detection method for epichlorohydrin in liquor, and as an auxiliary determination method for the addition of synthetic glycerol in liquor. Methods Epichlorohydrin in liquor was extracted and condensed by dichloromethane, separated by high elastic quartz capillary column, and determined by gas chromatography-mass spectrometer(GC-MS). The ion pair with the highest sensitivity was used for the quantitative analysis. Results The relative standard deviations(RSDs) of method were less than 10%, the recovery rates were 75.5%-89.0%, and the limit of detection was 1.0 μg/L. Conclusion This method is sensitive and accurate, which is suitable for the determination of epichlorohydrin in liquor.
Objective To establish a perfect and accurate detection method for epichlorohydrin in liquor, and as an auxiliary determination method for the addition of synthetic glycerol in liquor. Methods Epichlorohydrin in liquor was extracted and condensed by dichloromethane, separated by high elastic quartz capillary column, and determined by gas chromatography-mass spectrometer(GC-MS). The ion pair with the highest sensitivity was used for the quantitative analysis. Results The relative standard deviations(RSDs) of method were less than 10%, the recovery rates were 75.5%-89.0%, and the limit of detection was 1.0 μg/L. Conclusion This method is sensitive and accurate, which is suitable for the determination of epichlorohydrin in liquor.
引文
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[5]张国英,郭忠鹏,张梁,等.甘油代谢对酿酒酵母酒精发酵的影响[J].酿酒科技,2008,8(170):20-24.Zhang GY,Guo ZP,Zhang L,et al.Effects of glycerol metabolism on ethanol fermentation by industrial Saccharomyces cerevisiae[J].Liquor-Mak Sci Technol,2008,8(170):20-24.
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[11]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.Zhu JY,Du JH,Wang XJ,et al.Glycerin formation in wine and its influencing factors[J].Liquor Mak,2010,37(2):23-27.
[12]王宏华,蒋爱英,刘振胜.啤酒酿造过程中甘油的变化规律[J].酿酒科技,2015,2(248):62-64.Wang HH,Jiang AY,Liu ZS.The change rules of glycerol content in beer brewing[J].Liquor-Making Sci Technol,2015,2(248):62-64.
[13]大森俊郎,小川清.大麦烧酒醒中甘油的来源及其构成[J].酿酒科技,1995,6(72):82.Dasen JL,Xiao CQ.Origin and composition of glycerin in barley waking[J].Liquor-Mak Sci Technol,1995,6(72):82.
[14]孙筱萍,袁雅文.固相萃取-气相色谱质谱法测定水中环氧氯丙烷[J].河南预防医学杂志,2018,29(9):669-670Sun XP,Yuan YW.Determination of epichloropropane in water by solid phase extraction-gas chromatography[J].Henan J Prev Med,2018,29(9):669-670.
[15]李旭霞.液液萃取-气相色谱法测定水中环氧氯丙烷[J].能源与环境,2018,(3):77-78.Li XX.Determination of epichloropropane in water by liquid extraction and gas chromatography[J].Energy Environ,2018,(3):77-78.
[16]甘平胜,黄聪,朱惠扬,等.吹扫捕集/三重四极串联四极杆气质联用法测定饮用水中环氧氯丙烷[J].华南预防医学,2015,41(5):477-478.Gan PS,Huang C,Zhu HY,et al.Determination of epichlorohydrin in drinking water by purge-trap/triple quadrupole tandem quadrupole gas chromatography-mass spectrometry[J].South China J Prev Med,2015,41(5):477-478.
[17]GB/T 10781.1-2006浓香型白酒[S].GB/T 10781.1-2006 Strong flavour Chinese spirits[S].
[18]GB/T 10781.2-2006清香型白酒[S].GB/T 10781.2-2006 Mild flavour Chinese spirits[S].
[19]GB/T 10781.3-2006米香型白酒[S].GB/T 10781.3-2006 Rice flavour Chinese spirits[S].
[20]GB/T 20823-2017特香型白酒[S].GB/T 20823-2017 Te xiang xin Chinese spirits[S].
[21]GB/T 23547-2009浓酱兼香型白酒[S].GB/T 23547-2009 Nongjiang-flavour Chinese spirits[S].
[22]GB/T 26760-2011酱香型白酒[S].GB/T 26760-2011 Jiang-flavour Chinese spirits[S].
[2]稳定同位素比质谱技术在酒行业的应用[N].华夏酒报,2015,C48:1-3.Application of stable isotopic ratio mass spectrometry in wine industry[N].Huaxia Wine Newspaper,2015,C48:1-3.
[3]杨会.白酒中不挥发呈味有机酸和多羟基化合物研究[D].无锡:江南大学,2017.Yang H.Characterization of non-volatile gustatory organic acids and polyhydroxy compounds in Chinese liquors[D].Wuxi:Jiangnan University,2017.
[4]徐扬.几种酵母酒精及甘油等生成动力学研究[D].大连:大连工业大学,2011.Xu Y.Production kinetics of alcohol and glycerin in several yeasts[D].Dalian:Dalian Polytechnic University,2011.
[5]张国英,郭忠鹏,张梁,等.甘油代谢对酿酒酵母酒精发酵的影响[J].酿酒科技,2008,8(170):20-24.Zhang GY,Guo ZP,Zhang L,et al.Effects of glycerol metabolism on ethanol fermentation by industrial Saccharomyces cerevisiae[J].Liquor-Mak Sci Technol,2008,8(170):20-24.
[6]Christoph R,Schmidt B,Steinberner U,et al.Ullmann's encyclopedia of industrial chemistry[Z].2006.
[7]王军,杨鸿,张孟瑶.环氧氯丙烷下游产品生产现状及市场前景[J].氯碱工业,2004,(2):28-31.Wang J,Yang H,Zhang MY.Present production situation and market prospects of epichlorohydrin downstream products[J].Chlor-Alkali Ind,2004,(2):28-31.
[8]楼亨达.合成甘油工艺路线的探讨[J].化学世界,1964,(7):301-303.Lou HD.Discussion on the process route of synthetic glycerine[J].Chem World,1964,(7):301-303.
[9]Eric J,Walter HC,Neumann.Glycerine a key cosmetic ingredient[M].New York:Routledge,2018.
[10]沈伟.甘油的生产应用现状及技术开发新迚展[J].广州化工,2009,37(6):62-67.Shen W.Production and application of glycerol and its new utilization[J].Guangzhou Chem Ind,2009,37(6):62-67.
[11]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.Zhu JY,Du JH,Wang XJ,et al.Glycerin formation in wine and its influencing factors[J].Liquor Mak,2010,37(2):23-27.
[12]王宏华,蒋爱英,刘振胜.啤酒酿造过程中甘油的变化规律[J].酿酒科技,2015,2(248):62-64.Wang HH,Jiang AY,Liu ZS.The change rules of glycerol content in beer brewing[J].Liquor-Making Sci Technol,2015,2(248):62-64.
[13]大森俊郎,小川清.大麦烧酒醒中甘油的来源及其构成[J].酿酒科技,1995,6(72):82.Dasen JL,Xiao CQ.Origin and composition of glycerin in barley waking[J].Liquor-Mak Sci Technol,1995,6(72):82.
[14]孙筱萍,袁雅文.固相萃取-气相色谱质谱法测定水中环氧氯丙烷[J].河南预防医学杂志,2018,29(9):669-670Sun XP,Yuan YW.Determination of epichloropropane in water by solid phase extraction-gas chromatography[J].Henan J Prev Med,2018,29(9):669-670.
[15]李旭霞.液液萃取-气相色谱法测定水中环氧氯丙烷[J].能源与环境,2018,(3):77-78.Li XX.Determination of epichloropropane in water by liquid extraction and gas chromatography[J].Energy Environ,2018,(3):77-78.
[16]甘平胜,黄聪,朱惠扬,等.吹扫捕集/三重四极串联四极杆气质联用法测定饮用水中环氧氯丙烷[J].华南预防医学,2015,41(5):477-478.Gan PS,Huang C,Zhu HY,et al.Determination of epichlorohydrin in drinking water by purge-trap/triple quadrupole tandem quadrupole gas chromatography-mass spectrometry[J].South China J Prev Med,2015,41(5):477-478.
[17]GB/T 10781.1-2006浓香型白酒[S].GB/T 10781.1-2006 Strong flavour Chinese spirits[S].
[18]GB/T 10781.2-2006清香型白酒[S].GB/T 10781.2-2006 Mild flavour Chinese spirits[S].
[19]GB/T 10781.3-2006米香型白酒[S].GB/T 10781.3-2006 Rice flavour Chinese spirits[S].
[20]GB/T 20823-2017特香型白酒[S].GB/T 20823-2017 Te xiang xin Chinese spirits[S].
[21]GB/T 23547-2009浓酱兼香型白酒[S].GB/T 23547-2009 Nongjiang-flavour Chinese spirits[S].
[22]GB/T 26760-2011酱香型白酒[S].GB/T 26760-2011 Jiang-flavour Chinese spirits[S].