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作 者:杨红茹[1] 韩媛媛[1] 董玉平[1] 韩丹丹[1] 刘艳飞[1] 高文[1] 张博[1]
出 处:《中国卫生检验杂志》2013年第17期3419-3422,共4页Chinese Journal of Health Laboratory Technology
基 金:河北省科技厅指导计划(12275532);河北大学2012教改项目(JX07-Y-40);中-美合作项目:<减少有害饮酒全球行动-非商业酒饮用情况研究(中国-河北)>(2011-23)
摘 要:目的建立毛细管气相色谱柱测定白酒中甲醇、杂醇油等多种微量成分的方法,并以此对河北省内采集的65份自酿、散白酒酒样进行分析。方法毛细管色谱柱为DB—WAX(30m×0.32mm×0.25μm),乙酸正戊酯为内标,采用程序升温,检测器为氢火焰离子化检测器。以保留时间定性;以待测组分峰面积、待测物相对质量校正因子、内标物峰面积进行甲醇、杂醇油的定量。结果:本法在选定的色谱条件下,各种微量成分得到较好的分离,方法回收率在91%-96%之间,重现性好,准确度高,待测的6个组分在15min内全部显现;实验精密度RSD为0.4%~1.3%之间。65份自酿、散装白酒甲醇质量浓度均值为0.44±1.14g/L,总体合格率90.7%,6份超标酒样均来自家庭自酿白酒。结论本法快速简单,分离效果和实验精密度良好,适合同时测定酒中甲醇、杂醇油等微量成分。农村自酿白酒卫生质量欠佳,建议加强卫生监测。Objective To establish a rapid and sensitive method for determination of the trace methyl alcohol and fusel oil in alcohol by capillary gas chromatographic column, and analyze 65 samples of home - made and bulk liquor with this method. Methods DB - WAX(30 m × 0.32 mm ×0.25 μm) as chromatographic column, amyl acetate as internal standard, temperature programming and FID were involved in this determination. The methyl alcohol and fusel oil in the liquor samples were conducted qualitative analysis by retention time, and quantitative analysis by peak area, relative mass correction factors and internal standard substance peak area. Results Under the above conditions, all trace compositions were separated successfully within 15 minutes, with recoveries of 91% - 96% and good precision with RSD between 0.4% -1.3%. The qualified rate of metha- nol was 90.7% in 65 samples, and 6 over - limit samples were all from home - brewed liquor. Conclusion The method is simple and rapid, with high - degree separation efficiency and good precision, it is suitable for determination of methanol and fusel oil in liquor at the same time. The sanitary quality of rural brewed liquor is poor, suggesting the government should strengthen the health supervision and surveillance on home -made and bulk liquor in rural area in Hebei province.
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