米酒中6种醇的气相色谱外标法测定研究

摘要

为实现对米酒酿造过程中乙醇、正丙醇、异丁醇、异戊醇、己醇、β-苯乙醇的实时检测,建立用甲醇为溶剂,色谱柱为HP-INNOWAX、DB-FFAP、HP-5柱,同时测定米酒中6种醇类含量的气相色谱(GC)外标法.结果表明,以HP-INNOWAX为色谱柱,5倍甲醇稀释处理酒样;乙醇在0.15％vol～19.2％vol、高级醇在0.75～208 mg/L范围内呈线性相关(R2>0.999),定量限与检测限均<0.05 mg/L,重复性试验和精确度试验结果的相对标准偏差(RSD)均<5％;在添加高、中、低3个水平标准浓度下的平均回收率为90.89％～96.53％,相对标准偏差(RSD)为0.11％～3.02％.该方法样品处理简单,平行性好,准确度高,实用性强,同时降低对色谱柱的损耗,可用于粮食酒、果酒等酿造酒中乙醇及高级醇的检测.%To realize the real-time monitoring of ethanol, n-propyl alcohol, isobutanol, iso-amyl alcohol, hexanol and phenylethyl alcohol in the brewing process of rice wine, a method for the simultaneously determination of 6 alcohols contents in rice wine was established using methanol as solvent,HP-INNOWAX, DB-FFAP and HP-5 as chromatographic column by GC external standard method. The results showed that using HP-INNOWAX as chromatographic column, after wine sample treated with 5 times methanol dilution, the ethanol showed linear correlation between 0.15％vol-19.2％vol,and the higher alcohol within the range of 0.75-208 mg/L (R2>0.999). The quantitation limit and detection limit were both less than 0.05 mg/L. The relative standard deviation (RSD) of repeatability test and precision test was less than 5％. The average recovery rates of samples spiked in high, medium and low levels were 90.89％-96.53％, and the RSDs were 0.11％-3.02％. The method was simple to process the samples with good parallelism, high accuracy and practicability, and at the same time reduced the loss of the chromatographic column. It could be used for the detection of ethanol and higher alcohol in grain alcoholic drink and fruit wine in the future.