比色法测白酒中杂醇油含量方法优化及验证

Optimization and Validation of Colorimetric Method for Determination of Fusel Oil in Liquor

白酒中的杂醇油含量高低不仅影响酒体风格,还会引发“上头”现象,对人体健康产生危害。如何准确检测和有效降低白酒中杂醇油含量是白酒行业共同面对的难题。为提高分析的准确度,从国标中比色法测定白酒中杂醇油方法出发,通过控制变量和重复性试验得到一种稳定性良好、准确度高的试验方法。优化后试验方法为:酒样经过蒸馏预处理,取5 g/L的二甲氨基苯甲醛-硫酸溶液4 mL作为显色剂,100℃水浴30 min,1+1硫酸溶液作为稀释剂,摇匀后立即于波长494 nm处测定吸光值。该方法检出限为0.002 g/100mL;定量限为0.006 g/100mL;曲线线性为0.9996;精密度测试的相对标准偏差(以及变异系数CV)为0.016%,正确度测试的加标回收率为97.6%~101%。

The content of fusel oil in liquor not only affects the wine style,but also causes the"headache"phenomenon,which is harmful to human health.How to accurately detect and effectively reduce fusel oil content in liquor is a common problem faced by liquor industry.In order to improve the accuracy of analysis,a new method with good stability and high accuracy was obtained by controlling variable and repeatability test,which was based on the colorimetric method in national standard for the determination of fusel oil in liquor.The optimized test method was as follows:after the liquor sample was pretreated by distillation,4 mL of 5 g/L dimethylaminobenzaldehyd-sulfuric acid solution was taken as the color developer,100℃water bath for 30 min,1+1 sulfuric acid solution was used as the diluent,and the light absorption value was immediately measured at 494 nm wave length after shaking.The detection limit of this method was 0.002 g/100 mL.Limit of quantification was 0.006 g/100 mL;The linear curve was 0.9996.The relative standard deviation(RSD)and coefficient of variation(CV)of the precision test were 0.016%,and the recoveries of the accuracy test were 97.6%~101%.