涡旋辅助分散液液微萃取-气相色谱法测定清香型白酒中5种高级醇

采用涡旋辅助分散液液微萃取（DLLME）-气相色谱（GC）法测定清香型白酒中5种高级醇的含量。结果表明，最佳液液微萃取的提取条件为萃取剂二氯甲烷60 μL、分散剂丙酮100 μL、样品pH值5.5、酒精度15%vol、NaCl质量浓度0.19 g/mL、萃取时间30 s。在此优化条件下，正丙醇和异丁醇在含量为1.00～40.00 mg/L、异戊醇在含量为1.00～150.00 mg/L、2,3-丁二醇在含量为1.25～50.00 mg/L和β-苯乙醇在含量为0.25～10.00 mg/L的范围内具有较好的线性关系（R2＞0.99）；检出限分别为0.03 mg/L、0.01 mg/L、0.01 mg/L、0.02 mg/L和0.02 mg/L；精密度试验结果相对标准偏差（RSDs）＜7.0%，回收率为83.1%～108.3%。6种清香型白酒中正丙醇含量范围为0.064～0.116 g/L、异丁醇含量范围为0.057～0.127 g/L、异戊醇含量范围为0.262～0.450 g/L、2,3-丁二醇含量范围为0.017～0.035 g/L、β-苯乙醇含量范围为0.008～0.012 g/L。

Determination of 5 higher alcohols in light-flavor Baijiu by vortex-assisted dispersion liquid-liquid microextraction-gas chromatography

The contents of 5 higher alcohols in light-flavor Baijiu samples were detected by vortex-assisted dispersion liquid-liquid microextraction (DLLME) combined with GC. The results showed that the optimum liquid-liquid microextraction conditions were extraction solvent dichloromethane 60 μl, dispersant acetone 100 μl, sample pH value 5.5, alcohol content 15%vol, NaCl concentration 0.19 g/ml, and extraction time 30 s. Under the optimal conditions, the standard curves of n-propanol, isobutanol, isoamylol, 2,3-butanediol and β-phenylethanol had a good linearity (R2＞0.99) in the ranges of 1.00-40.00 mg/L, 1.00-40.00 mg/L, 1.00-150.00 mg/L, 1.25-50.00 mg/L and 0.25-10.00 mg/L, respectively. The detection limits were 0.03 mg/L, 0.01 mg/L, 0.01 mg/L, 0.02 mg/L, and 0.02 mg/L, respectively. The relative standard deviations (RSDs) of the precision tests results were all less than 7.0%, and the recoveries were 83.1%-108.3%. The contents of n-propanol, isobutanol, isoamylol, 2,3-butanediol and β-phenylethanol in 6 light-flavor Baijiu samples were 0.064-0.116 g/L, 0.057-0.127 g/L, 0.262-0.450 g/L, 0.017-0.035 g/L and 0.008-0.012 g/L, respectively.