气相色谱法测定白酒中醇类及酯类

Determination of alcohols and esters in liquor by gas chromatography

目的建立气相色谱法测定白酒中醇类和酯类的分析方法。方法样品前期处理简单,以叔戊醇为内标物,进行内标法标准曲线定量,采用FID氢火焰离子化检测器和毛细管色谱柱DB-FFAP(50m×0.32 mm, 0.50μm)及程序升温进行测定,检测器温度为300℃,进样口温度230℃,进样量0.5μL。结果各醇类及酯类混合标准溶液在相应的浓度范围内线性皆良好,相关系数r均大于0.999,检出限为3~9mg/L(S/N=3),定量限为10~30 mg/L (S/N=10),回收率为88.25%~98.75%,相对标准偏差(relative standard deviation,RSD)为2.75%~3.84%(n=6)。结论该方法简化了操作步骤,一次进样可以同时检测8种常规的醇类和酯类,提高工作效率和仪器的利用率,且回收率高,重现性和精密度良好,测定结果准确可靠,满足白酒中醇类和酯类含量的定量分析。

Objective To establish a method for the determination of alcohols and esters in liquor by gas chromatography.Methods The sample was pretreated simply,2-methyl-2-butanol was used as internal standard,the standard curve was quantified by internal standard method,and the sample was determined by flame ionization detector(FID),capillary column DB-FFAP(50 m×0.32 mm,0.50μm)and programmed temperature,the detector temperature was 300℃,the sample inlet temperature was 230℃,the sample volume was 0.5µL.Results The standard solutions of alcohols and esters had good linearity in the corresponding concentration range,the correlation coefficients r were greater than 0.999,the detection limits were 3‒9 mg/L(S/N=3),the quantitative limits were 10-30 mg/L(S/N=10),the recovery rates were 88.25%‒98.75%,relative standard deviations(RSDs)were 2.75%‒3.84%(n=6).Conclusion The method simplified the operation steps,one injection can detect 8 kinds of alcohol and ester at the same time,improve the work efficiency and the utilization rate of the instrument,with high recovery,good reproducibility and precision,the determination results are accurate and reliable,meet the alcohols and esters content in liquor of quantitative analysis.