CN1056235C - 一种用核磁共振波谱检测酒老熟程度的方法 - Google Patents

一种用核磁共振波谱检测酒老熟程度的方法 Download PDF

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CN1056235C
CN1056235C CN 94110246 CN94110246A CN1056235C CN 1056235 C CN1056235 C CN 1056235C CN 94110246 CN94110246 CN 94110246 CN 94110246 A CN94110246 A CN 94110246A CN 1056235 C CN1056235 C CN 1056235C
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CN1114048A (zh
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韩秀文
纪涛
胡皆汉
苏凡
刘秀梅
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Dalian Institute of Chemical Physics of CAS
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Abstract

一种用核磁共振波谱检测洒老熟程度的方法,包括样品准备、仪器调整、绘制谱图等步骤,其特征在于:谱图完成后,精确测量各谱峰半高宽度,确定待测酒的半高宽因子Δ1/2(OH)1/2(CHS),并与该类酒已经测定的标准进行比较,以确定待测酒的老化程度。本发明可以准确而可靠的检测酒的老熟程度。

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一种用核磁共振波谱检测酒老熟程度的方法
本发明涉及酒老熟程度的检测方法,特别是利用核磁共振波谱检测酒老熟程度的方法。
刚生产的新酒燥竦味,刺激性强,经老熟陈化后则口感柔和,回味绵长。酒老熟机是复杂,伴有物理和化学变化,如何判断其熟化程度乞今尚是个难题。目前除用色谱法检测成分外,国内外均依靠品酒师品尝法确定老熟程度和老熟后酒质的优劣。显然,品尝法难免受品酒师的健康状况及情绪好坏所左右,若能找到仪器分析检测方法,将会更方便客观地表征出真实情况。据文献报道,乙醇是刺激味觉的主要根源,老熟过程是乙醇与水分子缔合过程,缔合体降低了乙醇分子的浓度,随之降低辣味和刺激性,当缔合处于稳定状态即陈化达到终点。这一物理变化过程前人曾试图用′HNMR波谱化学位移来进行表征,但由于这种变化很小,未能达到目的。
本发明的目的在于提供一种利用核磁共振波谱检测酒老熟程度的方法,依据其可以可靠并准确地检测酒的老熟程度。
本发明提供了一种用核磁共振波谱检测酒老熟程度的方法,其特征在于检测步骤如下:(a)样品准备:用待测酒样清洗核磁样品管三次后,将待测酒样倒入样品管中;(b)仪器调试:匀场以保证良好的磁场均匀性;(c)采集谱图:把乙醇中甲基峰的化学位移定为1.16ppm,作为化学位移第二参考;画谱和积分曲线,精确测量各谱峰半高宽度;(d)数据处理:测定待测酒样的半高宽因子[Δ1/2(OH)/Δ1/2(CH3]的数值,与该类酒已经测定的标准进行比较,以确定待测酒的老熟程度。本发明采用′HNMR方法研究酒老熟程度,所引进的线宽因子Δ1/2(OH)/Δ1/2(CH3)成功地表征了酒在人工或者常规老熟过程中老熟的程度,得到的测试数据与品酒师品尝的结果吻合。当前,可作为品酒师品尝酒口感质量的辅助方法,当人们掌握了这种方法后,可望代替人工品尝的传统方法。下面通过实施例详述本发明。
附图1为1990.03.29测定的编号为04-0黑方威士忌′HNMR谱图。
实施例
实验仪器:日立R-24B型高分辨NMR波谱仪,样品Ф5mm,实验室恒温于24±1℃。
实验步骤:
1.样品管用乙醇清洗后,用蒸馏水冲洗干燥,确保样品管干净干燥;
2.小心倾侧酒样,用待测酒样润洗样品管三次,取酒样在样品内高度4~5mm,不加任何溶剂和参照物。
3.测试时认真仔细地匀均,保证良好的磁场均匀性,扫描时间150s,谱宽600Hz(10ppm),振幅2,积分幅值为7;
把乙醇中甲基的化学位移定为1.16ppm,作为化学位移的第二参考,画谱、积分曲线(不测乙醇、糖含量可不画积分曲线),再画放大谱图(见附图1)。
4.用读数显微镜精确测量各谱峰半高宽度(单位mm)。
5.测定待测酒的半高宽因子[Δ1/2(OH)1/2(CH3)]的数值,利用本实验积累的各种酒老熟过程至老熟终点的半宽因子数值与品尝结果的对应关系,即可得出老化程度。
表I和表II及表III为对几种酒的检测结果。
        表I人工老熟
              线宽因子1.马提尼味思美    2.042    1.9062.波酒            3.235    2.4343.兰带马爹利      1.752    1.313品酒师认为处理后口感大为提高。
        表II常规老熟
              线宽因子酒                 91年     93年1.汾酒            1.528    1.3822.国产白兰地      1.502    1.1403.竹叶青          1.954    1.708
    表III酒名    编   测  试       半高峰宽(mm)              线宽因子        备注
    号   时  间     Δ1/2(CH3)  Δ1/2(OH) Δ1/2(OH)1/2(CH3)白兰地  B6 91.06.27    3.412      4.922            1.443
        93.03.14    5.220      7.161            1.372竹叶青  原  90.03.22    2.348      5.699            2.427
    样  91.05.15    3.249      6.348            1.954古井    7# 90.05.29    3.271      4.441            1.358贡酒        91.05.10    3.683      4.787            1.300            老熟
        93.06.12    2.960      3.859            1.304            终点黑方威  04  90.03.29    3.412      6.208            1.819士忌    |   91.04.24    2.618      4.622            1.765
    0   93.06.03    3.240      4.311            1.326罗姆    013 90.03.23    2.201      3.357            1.525干酒    |   91.04.26    3.107      4.710            1.516
    1   93.06.02    2.680      3.860            1.440

Claims (1)

1.一种用核磁共振波谱检测酒老熟程度的方法,其特征在于检测步骤如下:
(a)样品准备:用待测酒样清洗核磁样品管三次后,将待测酒样倒入样品管中;
(b)仪器调试:匀场以保证良好的磁场均匀性;
(c)采集谱图:把乙醇中甲基峰的化学位移定为1.16ppm,作为化学位移第二参考;画谱和积分曲线,精确测量各谱峰半高宽度;
(d)数据处理:测定待测酒样的半高宽因子(Δ1/2(OH)/Δ1/2(CH3)]的数值,与该类酒已经测定的标准进行比较,以确定待测酒的老熟程度。
CN 94110246 1994-05-10 1994-05-10 一种用核磁共振波谱检测酒老熟程度的方法 Expired - Fee Related CN1056235C (zh)

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