芝麻香白酒中3-甲硫基丙醇的GC-FPD分析

建立了利用气相色谱-火焰光度检测器检测芝麻香白酒风味成分3-甲硫基丙醇的方法.样品前处理方法为CH2Cl2萃取,酒样浓缩50倍分析;色谱方法为DB-FFAP（60 m×0.25 mm×0.25μm）毛细管柱,程序升温,进样口温度为260℃,检测器温度为200℃;采用外标法定量.结果表明：在3-甲硫基丙醇质量浓度为5-100 mg/L时,线性相关系数为0.9913,检测限为2.5 mg/L,定量限为5 mg/L.在3-甲硫基丙醇质量浓度为8,30,80 mg/L 3个水平下,回收率为84.3%-89.7%,相对标准偏差为3.7%-4.6%.对国内5家芝麻香型白酒骨干生产企业共18个酒样的3-甲硫基丙醇经换算后的检测结果是：企业Ⅰ原酒及商品酒中均未检出3-甲硫基丙醇;企业Ⅱ原酒中未检出3-甲硫基丙醇,商品酒Ⅱ-a、Ⅱ-b、Ⅱ-c和Ⅱ-d中3-甲硫基丙醇质量浓度分别为1.03,0.35,0.80,0.67mg/L;企业Ⅲ原酒及商品酒中均未检出3-甲硫基丙醇;企业Ⅳ原酒及商品酒中3-甲硫基丙醇质量浓度低于0.1 mg/L;企业V原酒中未检出3-甲硫基丙醇,商品酒Ⅴ-a中3-甲硫基丙醇质量浓度为0.18 mg/L.

GC-FPD Analysis of 3-Methylthiopropanol in Sesame-Flavor Liquor

3-methylthiopropanol in Sesame-Flavor Liquor was analyzed by gas chromatography-flame photometric detector （GC-FPD） in this study. The wine was concentrated 50 times and extracted by dichloromethane for sample pretreatment. The chromatographic condition carried out that： polar chromatographic column DB-FFAP （60 m × 0.25 mm× 0.25 μm） , programmed temperature, inlet temperature 260 ℃ , detector temperature 200 ℃ External standard method was adopted. The results showed that with the concentration of 5 - 100 mg/L of 3-methylthiopropanol the linear correlation coefficient （ R2） was O. 991 3, LOD was 2.5 mg/L, LOQ was 5 mg/L, while with the level of 8,30,80 mg/L recovery rates were between 84.3% to 89.7% , R. S. D. ranged from 3.7% to 4.6%. Five major Sesame Flavor Liquor corporations and 18 samples were inspected. The 3-methylthiopropanol couldn＇t be detected in com- mercial wines including the corporation of Ⅰ and Ⅲ, original wines such as Ⅰ , Ⅱ ,Ⅲ and V. While the concentration of 3-methyhhiopropanol in the commercial wines of Ⅱ-a, Ⅱ-b, Ⅱ-c, II-d and V-a were 1.03, 0. 35, 0. 80, 0.67, 0. 18 mg/L, respectively. In the corporation of IV original wine and commercial wine, its concentration were all below 0. 1 mg/L.