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目的建立毛细管柱气相色谱内标法测定白酒中甲醇、杂醇油、酯类等11种成分的分析方法,以便快速、高效、准确的测定白酒中多种成分物质,满足日常检测工作的需要。方法利用气相色谱法,通过程序升温模式,以DBWAX柱(30 m×0.25μm×0.32 mm)为分离柱,火焰离子化检测器(FID)检测,以保留时间定性,乙酸正丁酯内标标准曲线法定量。结果 11种物质在0.02%~1.0%(V/V)线性范围内,相关系数≥0.998 9;样品加标回收率为90.0%~102%,精密度试验的相对标准偏差为0.11%~1.05%,方法检出限为0.001 g/L~0.010 g/L。结论该法操作简单、稳定可靠,实现了白酒中11种成分良好的分离效果和实验精密度,满足检测的要求,可以应用到日常白酒样品的检测分析中。
OBJECTIVE To establish a method for the determination of 11 constituents of methanol, fusel oil and esters in white spirit by capillary gas chromatography with internal standard method, in order to quickly, efficiently and accurately determine the contents of many components of liquor and meet the needs of routine testing. Methods Gas chromatography, temperature programmed mode, DBWAX column (30 m × 0.25 μm × 0.32 mm) as separation column and flame ionization detector (FID) were used to determine the retention time. The internal standard of n-butyl acetate Curve quantitative. Results The linearity of the 11 substances was in the range of 0.02% -1.0% (V / V), the correlation coefficient was ≥0.998 9. The spiked recoveries were 90.0% -102%. The relative standard deviations of the precision test were 0.11% -1.05% The detection limit was 0.001 g / L ~ 0.010 g / L. Conclusion The method is simple, stable and reliable, and has achieved the good separation effect and precision of 11 components in liquor to meet the testing requirements. It can be applied to the detection and analysis of daily liquor sample.