摘要
建立了一种高灵敏和高选择性检测芝麻香型白酒中3-甲硫基丙醇的气相色谱法。为解决传统检测方法(GC-FID法)灵敏度低、选择性差、对色谱条件要求苛刻的问题,利用火焰光度检测器(FPD)(配有硫滤光片)对含硫化合物具有特异性响应的特性,建立了一种简便、快捷、选择性的检测酒中3-甲硫基丙醇的方法(GC-FPD法)。结果表明,在3-甲硫基丙醇质量浓度为0.1~10.0 mg/L范围内,线性回归方程为y=583 476.1x~2+1 648 312x-310 670.0,相关系数为0.999 9;检出限0.03 mg/L,定量限0.1 mg/L。加标回收率试验结果的平均回收率为93.1%~104.6%,日内精密度相对标准偏差(RSD1)为3.2%~4.9%,日间精密度相对标准偏差(RSD2)为1.1%~2.1%。该方法准确度及精密度良好,能够满足白酒中3-甲硫基丙醇的检测要求。
A highly sensitive and selective gas chromatographic method for the determination of 3-methylthio propanol in sesame-flavor Baijiu(Chinese liquor) was developed. In order to solve the traditional GC-FID detection method of low sensitivity, poor selectivity, and chromatographic conditions demanding, a simple, fast and high selective GC-FPD method for detecting 3-methylthio propanol was established using flame photometric detector(equipped with a S filter) with the specific response of sulfur compounds. The results showed that: in the range of 3-methylthio propanol concentration 0.1-10.0 mg/L, the linear regression equation was: y=583 476.1x~2+1 648 312x-310 670.0, the correlation coefficient was 0.999 9, the detection limit was 0.03 mg/L, and the limit of quantitation was 0.1 mg/L. The average recovery rate of the test was 93.1%-104.6%, the relative standard deviation of within day precision(RSD1) was 3.2%-4.9%, inter day precision(RSD2) was 1.1%-2.1%. The method had good accuracy and precision, which can meet the requirement of 3-methylthiol propano determination in sesame-flavor Baijiu.
引文
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