气相色谱法同时测定清香型白酒中的甲醇乙酸乙酯和乳酸乙酯含量
2025-08-09原超
Simultaneous Determination of Methanol, Ethyl Acetate and Ethyl Lactate in Qingxiangxing Baijiu by Gas Chromatography
YUANChao (Changzhi General Inspection and Testing Centre, Changzhi O46oo0, China)
Abstract: The method for the simultaneous determination of methanol, ethyl acetate and ethyl lactate in Qingxiangxing Baijiuby gas chromatography was established. A mixed internal standard of tertamyl alcohol/n-amyl acetate was added to the sample of Qingxiangxing Baijiu,separatedby capilary column,determined by hydrogen flame ion detector,andquantifiedby peak area internal standard method.Theresults showed thatthechromatographic separation effect of this method was good,the linearity of the three targetcomponents within their respective concentration ranges was good, the sensitivity was high, the precision was 1.32% to 1.81% ,and the recovery rate of spiking was between 90.0% to 106.7% ,which was suitable for the simultaneous analysis and determination of three components in Qingxiangxing Baijiu.
Keywords: gas chromatography; Qingxiangxing Baijiu; methanol; ethyl acetate; ethyl lactate
清香型白酒作为我国白酒八大香型之一,以其入口绵甜、醇厚柔和、清爽甘洌的特点,深受广大酒友好评,成为京津晋冀豫蒙等地家庭聚餐、商务宴请的必备佳品。甲醇是清香型白酒生产过程中产生的内源性有害成分,甲醇含量超标对消费者危害极大,一直以来都是《国家食品安全监督抽检实施细则》中规定的必检项目[。乙酸乙酯和乳酸乙酯作为清香型白酒的主要呈味物质,其含量直接影响白酒质量与风格特征,也是白酒企业质量监控和相关部门风险监测的项目[2]。然而,目前的国家标准检测方法中,甲醇、乙酸乙酯和乳酸乙酯对应两种检测方法,且《食品安全国家标准食品中甲醇的测定》(GB5009.266—2016)[3]中线性范围没有覆盖定量限,《白酒分析方法》(GB/T10345—2022)[4中则缺少检出限和定量限,因此,本文针对国家标准方法进行优化,建立了气相色谱法同时测定清香型白酒中甲醇、乙酸乙酯和乳酸乙酯的方法。
1材料与方法
1.1材料与试剂
某品牌清香型白酒,购自某超市;水中甲醇(BW902608-10000-L, 10000μg⋅mL-1 )、乙醇中乙酸乙酯(BW900965-25000-C, 25 000μg⋅mL-1 )、乙醇中乳酸乙酯(BW902654-25000-C, 25000μg⋅mL-1 )、乙醇/水中叔戊醇/乙酸正戊酯混标(浓度均为20 000μg⋅mL-1 ),均购自坛墨质检标准物质中心;无水乙醇(色谱纯),美国赛默飞世尔公司;实验室用水为一级超纯水。
分析检测
1.2仪器与设备
GC-2010气相色谱仪,日本岛津公司;FinnpipetteF3 ( 10~100μL 、
)移液器,美国赛默飞世尔公司;VORTEX1漩涡振荡器,德国艾卡公司;Synergy超纯水机,德国密理博公司。
1.3 试验方法
1.3.1 混合标准工作液配制
分别吸取25、100、200、400、 600μL 和1000μL 水中甲醇( 10000μgmL-1 )、乙醇中乙酸乙酯……
