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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(30 m×0.32 mm×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15 min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±1.14 g/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 method for the determination of methanol, fusel oil and other trace elements in liquor by capillary gas chromatography (GC), and to analyze the 65 samples of brewed and casual liquor collected in Hebei Province. Methods capillary column DB-WAX (30 m × 0.32 mm × 0.25μm), n-amyl acetate as an internal standard, using the program temperature, the detector for the flame ionization detector. To retain the time qualitative; peak area to be measured, the relative mass correction factor, internal standard peak area of methanol, fusel oil quantitative. Results: Under the selected chromatographic conditions, various trace components were well separated. The recoveries were between 91% and 96%, reproducibility was good and the accuracy was high. Six components All appeared within 15 min; the experimental precision RSD was 0.4% ~ 1.3%. The mean concentration of methanol in 65 homemade and bulk white liquors was 0.44 ± 1.14 g / L, with an overall pass rate of 90.7%. Conclusion The method is rapid, simple, and the separation effect and experimental precision are good. It is suitable for the simultaneous determination of methanol, fusel oil and other trace elements in wine. The quality of rural home-brewed white wine is not good and health monitoring is recommended.