顶空气相色谱法测定葡萄酒中甲醇及市售葡萄酒质量调查

Determination of Methanol Content in Wine by Headspace Gas Chromatography and Survey on the Quality of Commercially Available Wine

建立了一种顶空-毛细管气相色谱快速测定葡萄酒中甲醇的方法。在75℃下振荡20 min后顶空进样，采用DB-wax毛细管柱（0.32μm，0.25 mm，30 m）和氢火焰检测器测定，内标法定量。结果表明，在16.4～821.0 mg/L范围内，甲醇的峰面积与其含量呈良好的线性关系，相关系数为0.999，平均回收率在99.85%～100.57%之间，样品重现性RSD在0.98%～2.44%之间，检出限为1.64 mg/L。该方法与国标GB/T 15038—2006方法相比更简便、高效，测定结果用配对t检验进行统计分析，在95%置信水平差异无统计学意义。对100批次武汉市售葡萄酒进行甲醇含量的调查分析，所有样品均检测出甲醇成分，其平均含量为157 mg/L，所有样品中甲醇含量均符合国家标准。

An analytical method for fast determination of methanol content in wine by headspace gas chromatography had been developed. Headspace sampling was performed after 20 min shaking at 75℃, then the measurement was carried out by FID detector after separation by DB-wax chromatographic column （0.32μm, 0.25 mm, 30 m） with internal standard method. The results suggested that, the linear range was be-tween 16.4 mg/L and 821.0 mg/L, the linear correlation coefficient was 0.999, the average recovery rate was between 99.85%and 100.57%, RSD was between 0.98%and 2.44%, and the detection limit was 1.64 mg/L. Compared with the method in GB/T 15038—2006, this method was more simple and efficient. The determination results were analyzed statistically by coupled t and there was no significant difference be-tween the two methods at the 95%confidence level. Finally, the methanol content of 100 batches of commercially available wine in Wuhan were detected and analyzed, and methanol was detected in all wine products and the average methanol content was 157 mg/L, which met nation-al standards.