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建立了利用气相色谱-质谱/选择离子扫描法(GC-MS/SIM)检测芝麻香白酒特征成分3-甲硫基丙醇的方法。样品前处理方法:CH2Cl2萃取、酒样浓缩5倍分析;色谱方法:DB-FFAP(60 m×0.25 mm×0.25μm)毛细管柱,程序升温;SIM方法检测质荷比106和61的离子;采用外标法定量。结果表明:在3-甲硫基丙醇质量浓度为50μg/L~10 mg/L范围,线性回归方程:y=491995x+3561.7,线性相关系数为0.9991;检测限5μg/L,定量限10μg/L。在3-甲硫基丙醇质量浓度为80μg/L,800μg/L和8 mg/L 3个水平下,回收率在83.8%~114.1%之间,日内、日间精密度均小于5%。对5个品牌共21个酒样的3-甲硫基丙醇的检测结果显示:品牌1原酒及商品酒中均未检出3-甲硫基丙醇;品牌2原酒中未检出3-甲硫基丙醇;商品酒S-2-1、S-2-2、S-2-3和S-2-4中3-甲硫基丙醇含量分别为1.4,0.36,1.0,0.66 mg/L;品牌3原酒及商品酒中均未检出3-甲硫基丙醇;品牌4商品酒中未检出3-甲硫基丙醇,原酒中其含量为2.4μg/L;品牌5原酒中未检出3-甲硫基丙醇,商品酒S-5中3-甲硫基丙醇含量为0.24 mg/L。
A method for the determination of 3-methylthiopropanol, the characteristic component of sesame, by gas chromatography-mass spectrometry / selective ion scan (GC-MS / SIM) was established. Sample pretreatment: CH2Cl2 extraction, five times the wine sample concentration analysis; chromatographic method: DB-FFAP (60 m × 0.25 mm × 0.25μm) capillary column, programmed temperature; SIM method to detect the mass- External standard method. The results showed that the linear regression equation was y = 491995x + 3561.7, the linear correlation coefficient was 0.9991, the limit of detection was 5μg / L and the limit of quantification was 10μg / L when the concentration of 3-methylthiopropanol was 50μg / L ~ 10mg / L. The recoveries ranged from 83.8% to 114.1% at 3 levels of 3-methylthiopropanol at concentrations of 80μg / L, 800μg / L and 8mg / L. The intra- and inter-day precision was less than 5%. A total of 21 samples of 5 brands of 3-methylthiopropanol test results showed that: the brand of 1 original wine and wine are not detected in the 3-methyl mercaptan alcohol; brand 2 original wine was not detected 3- Methylthiopropanol; the content of 3-methylthiopropanol in commercial wine S-2-1, S-2-2, S-2-3 and S-2-4 were 1.4,0.36,1.0,0.66 mg / L; 3-methylthiopropanol was not detected in the original 3 brand wine and commercial wine; 3-methylmercaptopropanol was not detected in the brand 4 commercial wine, and its original content was 2.4 μg / L; brand 5 No 3-methylthiopropanol was detected in the original wine, and the content of 3-methylthiopropanol in commercial wine S-5 was 0.24 mg / L.