芝麻香型白酒中3-甲硫基丙醇的GC-FPD检测方法研究
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摘要
建立了一种高灵敏和高选择性检测芝麻香型白酒中3-甲硫基丙醇的气相色谱法。为解决传统检测方法(GC-FID法)灵敏度低、选择性差、对色谱条件要求苛刻的问题,利用火焰光度检测器(FPD)(配有硫滤光片)对含硫化合物具有特异性响应的特性,建立了一种简便、快捷、选择性的检测酒中3-甲硫基丙醇的方法(GC-FPD法)。结果表明,在3-甲硫基丙醇质量浓度为0.1~10.0 mg/L范围内,线性回归方程为y=583 476.1x~2+1 648 312x-310 670.0,相关系数为0.999 9;检出限0.03 mg/L,定量限0.1 mg/L。加标回收率试验结果的平均回收率为93.1%~104.6%,日内精密度相对标准偏差(RSD1)为3.2%~4.9%,日间精密度相对标准偏差(RSD2)为1.1%~2.1%。该方法准确度及精密度良好,能够满足白酒中3-甲硫基丙醇的检测要求。
A highly sensitive and selective gas chromatographic method for the determination of 3-methylthio propanol in sesame-flavor Baijiu(Chinese liquor) was developed. In order to solve the traditional GC-FID detection method of low sensitivity, poor selectivity, and chromatographic conditions demanding, a simple, fast and high selective GC-FPD method for detecting 3-methylthio propanol was established using flame photometric detector(equipped with a S filter) with the specific response of sulfur compounds. The results showed that: in the range of 3-methylthio propanol concentration 0.1-10.0 mg/L, the linear regression equation was: y=583 476.1x~2+1 648 312x-310 670.0, the correlation coefficient was 0.999 9, the detection limit was 0.03 mg/L, and the limit of quantitation was 0.1 mg/L. The average recovery rate of the test was 93.1%-104.6%, the relative standard deviation of within day precision(RSD1) was 3.2%-4.9%, inter day precision(RSD2) was 1.1%-2.1%. The method had good accuracy and precision, which can meet the requirement of 3-methylthiol propano determination in sesame-flavor Baijiu.
A highly sensitive and selective gas chromatographic method for the determination of 3-methylthio propanol in sesame-flavor Baijiu(Chinese liquor) was developed. In order to solve the traditional GC-FID detection method of low sensitivity, poor selectivity, and chromatographic conditions demanding, a simple, fast and high selective GC-FPD method for detecting 3-methylthio propanol was established using flame photometric detector(equipped with a S filter) with the specific response of sulfur compounds. The results showed that: in the range of 3-methylthio propanol concentration 0.1-10.0 mg/L, the linear regression equation was: y=583 476.1x~2+1 648 312x-310 670.0, the correlation coefficient was 0.999 9, the detection limit was 0.03 mg/L, and the limit of quantitation was 0.1 mg/L. The average recovery rate of the test was 93.1%-104.6%, the relative standard deviation of within day precision(RSD1) was 3.2%-4.9%, inter day precision(RSD2) was 1.1%-2.1%. The method had good accuracy and precision, which can meet the requirement of 3-methylthiol propano determination in sesame-flavor Baijiu.
引文
[1]高传强.芝麻香型白酒风味物质及其生物活性研究[D].武汉:湖北工业大学,2017.
[2]蔡鹏飞,邵传贞,张娜,等.芝麻香白酒特征风味物质的猜想[J].酿酒,2014,41(5):76-78.
[3]黄忠白,丁媛,黄健,等.栉孔扇贝柱和扇贝裙边中挥发性物质的比较分析[J].食品科学,2016,37(4):98-102.
[4]贺书珍,初众,谭乐和,等.不同酵母发酵对菠萝蜜果酒香气成分的影响[J].热带农业科学,2017,37(9):76-82.
[5]PINO J A,QUERIS O.Characterization of odor-active compounds in Guava wine[J].J Agr Food Chem,2011,59(9):4885-4890.
[6]FANG Y,QIAN M C.Sensitive quantification of sulfur compounds in wine by headspace solid-phase microextraction technique[J].J Chromatogr A,2005,1080(2):177-185.
[7]WELDEGERGIS B T,CROUCH A M,GORECKI T,et al.Solid phase extraction in combination with comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry for the detailed investigation of volatiles in South African red wines[J].Anal Chim Acta,2011,701(1):98-111.
[8]国家质量监督检验检疫总局.GB 20824—2007《芝麻香型白酒》[S].北京:中国标准出版社,2007.
[9]国家质量监督检验检疫总局.GB/T 10345—2007《白酒分析方法》[S].北京:中国标准出版社,2007.
[10]孙啸涛,张锋国,董蔚,等.芝麻香白酒中3-甲硫基丙醇的GC-FPD分析[J].食品科学技术学报,2014,32(5):27-34.
[11]万素琴,周玮,颜春荣,等.GC-MS法测定芝麻香型白酒中3-甲硫基丙醇含量[J].江苏农业科学,2014,42(4):268-270.
[12]孙啸涛,张锋国,董蔚,等.GC-MS/SIM法测定芝麻香型白酒中3-甲硫基丙醇[J].中国食品学报,2015,15(2):215-221.
[13]赵东瑞,柳金龙,张锋国,等.GC-MS/SIM内标法定量分析两种类型酒中的3-甲硫基丙醇[J].中国食品学报,2016,5(16):196-204.
[14]唐晖慧,金美东.分散液液微萃取结合气相色谱-火焰光度检测器法测定芝麻香型白酒中3-甲硫基丙醇[J].食品与发酵工业,2016,42(5):210-216.
[15]张小溪,王成涛,安晶晶,等.发酵液中3-甲硫基丙醇的GC-MS分析[J].中国酿造,2013,32(3):146-151.
[16]程伟,彭兵,谢国排,等.浓香型白酒高温堆积粮醅中挥发性风味物质的检测分析[J].酿酒,2017,44(4):28-33.
[17]钟伟燕,尹万江,李行方,等.GC-FPD测定二硫化碳的计算方法及用于空气检测的探讨[J].职业与健康,2013,15(29):1903-0908.
[18]武汉大学.分析化学(下册)[M].北京:高等教育出版社,2014:525-526.
[2]蔡鹏飞,邵传贞,张娜,等.芝麻香白酒特征风味物质的猜想[J].酿酒,2014,41(5):76-78.
[3]黄忠白,丁媛,黄健,等.栉孔扇贝柱和扇贝裙边中挥发性物质的比较分析[J].食品科学,2016,37(4):98-102.
[4]贺书珍,初众,谭乐和,等.不同酵母发酵对菠萝蜜果酒香气成分的影响[J].热带农业科学,2017,37(9):76-82.
[5]PINO J A,QUERIS O.Characterization of odor-active compounds in Guava wine[J].J Agr Food Chem,2011,59(9):4885-4890.
[6]FANG Y,QIAN M C.Sensitive quantification of sulfur compounds in wine by headspace solid-phase microextraction technique[J].J Chromatogr A,2005,1080(2):177-185.
[7]WELDEGERGIS B T,CROUCH A M,GORECKI T,et al.Solid phase extraction in combination with comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry for the detailed investigation of volatiles in South African red wines[J].Anal Chim Acta,2011,701(1):98-111.
[8]国家质量监督检验检疫总局.GB 20824—2007《芝麻香型白酒》[S].北京:中国标准出版社,2007.
[9]国家质量监督检验检疫总局.GB/T 10345—2007《白酒分析方法》[S].北京:中国标准出版社,2007.
[10]孙啸涛,张锋国,董蔚,等.芝麻香白酒中3-甲硫基丙醇的GC-FPD分析[J].食品科学技术学报,2014,32(5):27-34.
[11]万素琴,周玮,颜春荣,等.GC-MS法测定芝麻香型白酒中3-甲硫基丙醇含量[J].江苏农业科学,2014,42(4):268-270.
[12]孙啸涛,张锋国,董蔚,等.GC-MS/SIM法测定芝麻香型白酒中3-甲硫基丙醇[J].中国食品学报,2015,15(2):215-221.
[13]赵东瑞,柳金龙,张锋国,等.GC-MS/SIM内标法定量分析两种类型酒中的3-甲硫基丙醇[J].中国食品学报,2016,5(16):196-204.
[14]唐晖慧,金美东.分散液液微萃取结合气相色谱-火焰光度检测器法测定芝麻香型白酒中3-甲硫基丙醇[J].食品与发酵工业,2016,42(5):210-216.
[15]张小溪,王成涛,安晶晶,等.发酵液中3-甲硫基丙醇的GC-MS分析[J].中国酿造,2013,32(3):146-151.
[16]程伟,彭兵,谢国排,等.浓香型白酒高温堆积粮醅中挥发性风味物质的检测分析[J].酿酒,2017,44(4):28-33.
[17]钟伟燕,尹万江,李行方,等.GC-FPD测定二硫化碳的计算方法及用于空气检测的探讨[J].职业与健康,2013,15(29):1903-0908.
[18]武汉大学.分析化学(下册)[M].北京:高等教育出版社,2014:525-526.