CN113791144A - 利用高效气相色谱检测白酒中手性乳酸乙酯的方法 - Google Patents
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Abstract
本发明属于白酒检测技术领域,具体涉及利用高效气相色谱检测白酒中手性乳酸乙酯的方法,手性乳酸乙酯包括L‑乳酸乙酯和D‑乳酸乙酯;酒样无需进行前处理,采安捷伦手性毛细管柱:19091G‑B233‑30mX0.25mmX0.25um,直接进样,样品经该色谱柱分离后,采用氢火焰检测器进行检测。本发明方法简单快捷,能够准确地对白酒中的乳酸乙酯进行定性、定量,为白酒中两种手性乳酸乙酯的准确判定、快速检测提供科学依据,为区分天然发酵乳酸乙酯与人为添加乳酸乙酯提供新思路。
Description
技术领域
本发明属于白酒检测技术领域,具体涉及利用高效气相色谱检测白酒中手性乳酸乙酯的方法。
背景技术
随着分析检测技术的不断发展,特别是高效毛细管气相色谱、液相色谱以及气质、液质联用技术的发展和应用,结合白酒的感官品尝、探明白酒中骨架成分的种类以及含量,研究其组成特点,有可能逐步揭开各类名酒“独特风味”的奥秘。众多研究人员在试图努力采用最新技术去识别未曾认识的白酒中微量成分甚至痕量成分,以对白酒的风格特色做出判定区别。
现有技术中的检测方法不便于对酒中的乳酸乙酯进行定量与定性的检测,并且检测方式较为复杂。
发明内容
本发明的目的在于提供利用高效气相色谱检测白酒中手性乳酸乙酯的方法,解决了现有技术中的检测方法不便于对酒中的乳酸乙酯进行定量与定性的检测,并且检测方式较为复杂的问题。
为了达到上述目的,本发明提供利用高效气相色谱检测白酒中手性乳酸乙酯的方法,
所述手性乳酸乙酯包括L-乳酸乙酯和D-乳酸乙酯:
所用仪器为:Agilent7890A气相色谱仪、配备安捷伦手性毛细管柱:19091G-B233-30mX0.25mmX0.25um、G4513A自动进样器、7693Autosampler 150位盘、G2171BA化学工作站、氢火焰检测器;
所述方法包括如下步骤:
(1)无需对酒样进行处理;
使用G4513A自动进样器对酒样进行取样0.5uL,放入到Agilent7890A气相色谱仪内进行分离:
(2)设定Agilent7890A气相色谱仪的条件:
色谱柱:安捷伦手性毛细管柱:19091G-B233-30mX0.25mmX0.25um,色谱仪用载气为高纯氮气,柱温70℃;
样品室温度:10-20℃;
流动相:A相为氮气,B相为酒样,然后进行程序升温,进样量为0.5uL,所检测时间为14Min,分流比为25:1,恒定流速为1mL/min;
(3)采用氢火焰检测器进行检测;
将待测酒样按照步骤(1)的方式进行处理后,按步骤(2)与步骤(3)得方式进行检测,然后通过G2171BA化学工作站计算峰值面积进行定性与定量。
进一步,所述步骤(2)中的程序升温方法为:
初始温度为70℃,保持8min,再以40℃/min快速升温到220℃,保持6min。
进一步,所述步骤(3)的具体方法为:
取L-乳酸乙酯和D-乳酸乙酯配制质量浓度范围在12.5~300μg/L的混合系列标准工作溶液,然后按照(2)所设定的条件取0.5uL各标准工作溶液进样,作超高效气相色谱检测,以待测物的峰面积对其所相应的质量浓度进行线性回归,获得两种手性乳酸乙酯的线性回归方程,各线性回归方程所对应的曲线,即为相应手性乳酸乙酯的标准曲线;
待测白酒酒样的检测将待测白酒酒样按步骤(1)的方式进行前处理后,取1.5mL按步骤(2)的条件作FID检测,通过收集放大,获得待测样品的色谱图,获得待测样品的色谱图,对待测白酒酒样根据保留时间进行定性分析,然后根据标准曲线对待测白酒酒样进行定量分析。
本发明的有益效果在于:方法简单快捷,能够准确地对白酒中的乳酸乙酯进行定性、定量,为白酒中两种手性乳酸乙酯的准确判定、快速检测提供科学依据,为区分天然发酵乳酸乙酯与人为添加乳酸乙酯提供新思路。
附图说明
图1为本发明实施例利用高效气相色谱检测白酒中手性乳酸乙酯的方法的初温分离乳酸乙酯对映体色谱图;
图2为本发明实施例利用高效气相色谱检测白酒中手性乳酸乙酯的方法的升温分离乳酸乙酯对映体色谱图。
具体实施方式
下面通过具体实施方式进一步详细说明:
如图1、图2所示,本实施例提供利用高效气相色谱检测白酒中手性乳酸乙酯的方法,
所述手性乳酸乙酯包括L-乳酸乙酯和D-乳酸乙酯:
所用仪器为:Agilent7890A气相色谱仪、配备安捷伦手性毛细管柱:19091G-B233-30mX0.25mmX0.25um、G4513A自动进样器、7693Autosampler 150位盘、G2171BA化学工作站、氢火焰检测器;
所述方法包括如下步骤:
(1)无需对酒样进行处理;
使用G4513A自动进样器对酒样进行取样0.5uL,放入到Agilent7890A气相色谱仪内进行分离:
(2)设定Agilent7890A气相色谱仪的条件:
色谱柱:安捷伦手性毛细管柱:19091G-B233-30mX0.25mmX0.25um,色谱仪用载气为高纯氮气,柱温70℃;
样品室温度:10-20℃;
流动相:A相为氮气,B相为酒样,然后进行程序升温,进样量为0.5uL,所检测时间为14Min,分流比为25:1,恒定流速为1mL/min;
(3)采用氢火焰检测器进行检测;
将待测酒样按照步骤(1)的方式进行处理后,按步骤(2)与步骤(3)得方式进行检测,然后通过G2171BA化学工作站计算峰值面积进行定性与定量。
所述步骤(2)中的程序升温方法为:
初始温度为70℃,保持8min,再以40℃/min快速升温到220℃,保持6min。
所述步骤(3)的具体方法为:
取L-乳酸乙酯和D-乳酸乙酯配制质量浓度范围在12.5~300μg/L的混合系列标准工作溶液,然后按照(2)所设定的条件取1.5mL各标准工作溶液进样,作超高效气相色谱检测,以待测物的峰面积对其所相应的质量浓度进行线性回归,获得两种手性乳酸乙酯的线性回归方程,各线性回归方程所对应的曲线,即为相应手性乳酸乙酯的标准曲线;
气相色谱的每一个峰面积都对映相应物质含量,安捷伦G2171BA化学工作站可以直接计算出峰面积PA*S值,我们可以根据对映体峰面积求算出左右旋体相对百分含量以及百分比差ee值(对应旋光度),如下表:
白酒样品与香料物质在色谱分析中乳酸乙酯对映体面积百分含量以及百分比差表
待测白酒酒样的检测将待测白酒酒样按步骤(1)的方式进行前处理后,取1.5mL按步骤(2)的条件作UPC2检测,通过使用3D波长扫描,获得待测样品的色谱图,对待测白酒酒样根据保留时间进行定性分析,然后根据标准曲线对待测白酒酒样进行定量分析。
本发明具体实施过程如下:以上为我们在市场上购买的乳酸乙酯香料与一部份白酒,还有一些是剑南春基础酒与成品酒,虽然数据有限,但我们发现一个有趣的规律,我们分析的几个市场上的香料均为左旋,且往往百分比差ee值较高,而我们确认的固态发酵酒往往右旋,ee值在15~37%之间,我们采用香料勾兑的白酒均为左旋,且随着1#2#3#勾兑酒样添加的香料越多,左旋ee值越高,而市场上购买的白酒大多为右旋,且ee值各不相同,仅个别低档酒如12#与16#为左旋,于是我们得出结论:纯粮固态发酵白酒乳酸乙酯均为右旋,香料的添加会严重影响乳酸乙酯对映体比例的改变,我们不能判定添加了香料就一定左旋,但乳酸乙酯左旋的白酒一定添加了香料。乳酸乙酯对白酒风味有着重要影响,这是毋庸置疑的,但乳酸乙酯对映体含量比例,其ee值对风味形成的影响。
需要提前说明的是,在本发明中,除非另有明确的规定和限定,术语“安装”、“相连”、“连接”、“固定”等术语应做广义理解,例如,可以是固定连接,也可以是可拆卸连接,或一体地连接;可以是直接相连,也可以通过中间媒介间接相连,可以是两个元件内部的连通。对于本领域的普通技术人员而言,可以根据具体情况理解上述术语在本发明中的具体含义。
以上所述的仅是本发明的实施例,方案中公知的具体结构及特性等常识在此未作过多描述。应当指出,对于本领域的技术人员来说,在不脱离本发明结构的前提下,还可以作出若干变形和改进,这些也应该视为本发明的保护范围,这些都不会影响本发明实施的效果和专利的实用性。本申请要求的保护范围应当以其权利要求的内容为准,说明书中的具体实施方式等记载可以用于解释权利要求的内容。
Claims (3)
1.利用高效气相色谱检测白酒中手性乳酸乙酯的方法,其特征在于:
所述手性乳酸乙酯包括L-乳酸乙酯和D-乳酸乙酯:
所用仪器为:Agilent7890A气相色谱仪、配备安捷伦手性毛细管柱:19091G-B233-30mX0.25mmX0.25um、G4513A自动进样器、7693Autosampler 150位盘、G2171BA化学工作站、氢火焰检测器;
所述方法包括如下步骤:
(1)无需对酒样进行处理;
使用G4513A自动进样器对酒样进行取样0.5uL,放入到Agilent7890A气相色谱仪内进行分离:
(2)设定Agilent7890A气相色谱仪的条件:
色谱柱:安捷伦手性毛细管柱:19091G-B233-30mX0.25mmX0.25um,色谱仪用载气为高纯氮气,柱温70℃;
样品室温度:10-20℃;
流动相:A相为氮气,B相为酒样,然后进行程序升温,进样量为0.5uL,所检测时间为14Min,分流比为25:1,恒定流速为1mL/min;
(3)采用氢火焰检测器进行检测;
将待测酒样按照步骤(1)的方式进行处理后,按步骤(2)与步骤(3)得方式进行检测,然后通过G2171BA化学工作站计算峰值面积进行定性与定量。
2.根据权利要求1所述的利用高效气相色谱检测白酒中手性乳酸乙酯的方法,其特征在于:所述步骤(2)中的程序升温方法为:
初始温度为70℃,保持8min,再以40℃/min快速升温到220℃,保持6min。
3.根据权利要求1所述的利用高效气相色谱检测白酒中手性乳酸乙酯的方法,其特征在于:所述步骤(3)的具体方法为:
取L-乳酸乙酯和D-乳酸乙酯配制质量浓度范围在12.5~300μg/L的混合系列标准工作溶液,然后按照(2)所设定的条件取1.5mL各标准工作溶液进样,作超高效气相色谱检测,以待测物的峰面积对其所相应的质量浓度进行线性回归,获得两种手性乳酸乙酯的线性回归方程,各线性回归方程所对应的曲线,即为相应手性乳酸乙酯的标准曲线;
待测白酒酒样的检测将待测白酒酒样按步骤(1)的方式进行前处理后,取1.5mL按步骤(2)的条件作FID检测,通过收集放大,获得待测样品的色谱图,对待测白酒酒样根据保留时间进行定性分析,然后根据标准曲线对待测白酒酒样进行定量分析。
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