GC-MS法同时快速测定酒精中9种醇类化合物的含量
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摘要
为准确测定酒精中杂醇类化合物含量,采用气相色谱-质谱联用仪(GC-MS),DB-624毛细管柱直接进样,氘代-1-丙醇-1,1,3,3,3-d5为内标,20:1分流进样,进样量1μL,程序升温,质谱扫描范围:29～300 m/z;SIM扫描模式建立了一种快速测定酒精中9种醇类化合物含量的方法。研究了方法的色谱条件、内标物选择、样品前处理等因素对检测结果的影响,并对条件予以优化。在优化的条件下,9种醇类化合物在0.2～10 mg/L内有很好的线性范围,相关系数均在0.993以上,定量限在0.60～0.85 mg/kg之间,加标实验的平均回收率在89.4%～105.2%之间,相对标准偏差(RSD)在1.89%～4.28%之间,结果表明该方法简便、快速、准确,适用于酒精中9种杂醇类化合物的同时分析测定。
To measure the content of alcoholic compounds in the alcohol in a more accurate and rapid way, a method was established with gas chromatography-mass spectrometry by ion scanning which was used to simultaneously determine the content of 9 alcohol compounds in alcohol, the method using DB-624 capillary column injection and deuterated 1-propanol-1,1,3,3,3-d5 as internal standard. Split sampling with the ratio of20:1 and the volume of 1μL is adopted. Temperature rise is controlled by the program and MS scanning range is controlled at 29-300 m/z. As a result, a method for rapidly determining 9 alcoholic compounds in the alcohol is established under the selective ion monitoring(SIM) scanning mode. The impacts of the chromatographic conditions, selection of internal standard, pre-treatment of samples and other factors on the detection results are analyzed and optimized in this paper. Under the optimized conditions,9 kinds of alcohol compounds have good linear range in 0.2-10 mg/L, the correlation coefficient is above 0.993, the limit of quantification is between0.60 and 0.85 mg/kg, the average recovery rate of spiked experiment is 89.4%-105.2%, the relative standard deviation was between 1.89% and 4.28%. The experimental results show that the method is simple, rapid and accurate. It is suitable for simultaneous determination of 9 alcohol compounds in alcohol.
To measure the content of alcoholic compounds in the alcohol in a more accurate and rapid way, a method was established with gas chromatography-mass spectrometry by ion scanning which was used to simultaneously determine the content of 9 alcohol compounds in alcohol, the method using DB-624 capillary column injection and deuterated 1-propanol-1,1,3,3,3-d5 as internal standard. Split sampling with the ratio of20:1 and the volume of 1μL is adopted. Temperature rise is controlled by the program and MS scanning range is controlled at 29-300 m/z. As a result, a method for rapidly determining 9 alcoholic compounds in the alcohol is established under the selective ion monitoring(SIM) scanning mode. The impacts of the chromatographic conditions, selection of internal standard, pre-treatment of samples and other factors on the detection results are analyzed and optimized in this paper. Under the optimized conditions,9 kinds of alcohol compounds have good linear range in 0.2-10 mg/L, the correlation coefficient is above 0.993, the limit of quantification is between0.60 and 0.85 mg/kg, the average recovery rate of spiked experiment is 89.4%-105.2%, the relative standard deviation was between 1.89% and 4.28%. The experimental results show that the method is simple, rapid and accurate. It is suitable for simultaneous determination of 9 alcohol compounds in alcohol.
引文
[1]王珍,周洋,李春丽,等.浅谈白酒中杂醇油的分析方法[J].酿酒科技,2017,276(6):77-79.
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[12]吴林芬,杨光宇,胡秋芬,等.气相色谱法测定食用酒精中甲醇和杂醇油的含量[J].云南民族大学学报(自然科学版),2012,21(4):252-255.
[13]邓青,邓岚,荆碧.毛细管气相色谱快速测定白酒中甲醇[J].云南师范大学学报(自然科学版),2002,22(5):42-43.
[14]王斌,冯锡凯,马立明.气相色谱内标(环己烷)法测定蒸馏酒中甲醇、杂醇油含量[J].中国卫生检验杂志,2006,16(7):802-803.
[15]石相莉,邓全道.酒中甲醇、杂醇油、乙酸乙酯、己酸乙酯的检测[J].中国卫生检验杂志,2007,17(11):2107-2113.
[16]邹志辉,张艳林,苑丽红.气相色谱法测定自酒中甲醇及杂油醇含量的探讨[J].贵州农业科学,2008,36(2):158-159.
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[18]李超,段海波,范多青,等.固相萃取-气质联用法同时快速测定水性胶黏剂中16种邻苯二甲酸酯[J].分析试验室,2014,33(5):592-596.
[2]孙伟,汪清美.气相色谱法测定白酒中的甲醇和杂醇油[J].信阳农业高等专科学校学报,2014,24(2):109-111.
[3]李珍,杨洋.改良气相色谱分析法分离测定11种杂醇油[J].食品安全导刊,2017(33):74-75.
[4]彭清涛,王力.毛细管气相色谱法同时测定白酒中的甲醇和杂醇油[J].化学分析计量,2007(1):33-34.
[5]湛社霞,卢佑演,张宏,等.蒸馏酒中甲醇和杂醇油测定的色谱条件优化[J].中国卫生检验杂志,2011,21(8):1944-1946.
[6]洪薇,符传武.气相色谱法同时测定白酒中的8种物质[J].中国酿造,2015(10):134-137.
[7]罗杰,敖宗华,王松涛,等.浓香型白酒不同类别基酒中杂醇油相关性研究[J].酿酒科技,2015(1):43-44.
[8]童永鑫,李玲,杨文宇,等.气相色谱法测定石榴葡萄酒中的甲醇和杂醇油[J].中国酿造,2013,32(3):142-145.
[9]熊道陵,李金辉,钟洪鸣.杂醇油提纯分离技术及应用[J].酿酒科技,2008(4):65-68.
[10]王立钊,梁慧珍,马树奎,等.影响固态发酵白酒中杂醇油生成因素的研究[J].酿酒科技,2006(5):43-45,48.
[11]陈丽娟,郭春芳.比色法测白酒中杂醇油含量方法探讨[J].酿酒,2009,28(5):71-72.
[12]吴林芬,杨光宇,胡秋芬,等.气相色谱法测定食用酒精中甲醇和杂醇油的含量[J].云南民族大学学报(自然科学版),2012,21(4):252-255.
[13]邓青,邓岚,荆碧.毛细管气相色谱快速测定白酒中甲醇[J].云南师范大学学报(自然科学版),2002,22(5):42-43.
[14]王斌,冯锡凯,马立明.气相色谱内标(环己烷)法测定蒸馏酒中甲醇、杂醇油含量[J].中国卫生检验杂志,2006,16(7):802-803.
[15]石相莉,邓全道.酒中甲醇、杂醇油、乙酸乙酯、己酸乙酯的检测[J].中国卫生检验杂志,2007,17(11):2107-2113.
[16]邹志辉,张艳林,苑丽红.气相色谱法测定自酒中甲醇及杂油醇含量的探讨[J].贵州农业科学,2008,36(2):158-159.
[17]延鑫.气相色谱法测定地方白酒中乙酸乙酯、杂醇油含量[J].北京联合大学学报(自然科学版),2009,23(3):53-56.
[18]李超,段海波,范多青,等.固相萃取-气质联用法同时快速测定水性胶黏剂中16种邻苯二甲酸酯[J].分析试验室,2014,33(5):592-596.