GC-MS/SIM法测定芝麻香型白酒中3-甲硫基丙醇  

Analysis of 3-Methylthiopropanol in Sesame Flavor Liquor by GC-MS/SIM

作　　者：孙啸涛[1,2] 张锋国 董蔚[1,2] 赵东瑞[1,2] 孙金沅[1,2] 孙宝国[1,2] 

机构地区：[1]北京工商大学北京市食品风味化学重点实验室,北京100048 [2]北京工商大学食品质量与安全北京实验室,北京100048 [3]山东扳倒井集团技术中心,山东高青256300

出　　处：《中国食品学报》2015年第2期214-222,共9页Journal of Chinese Institute Of Food Science and Technology

基　　金：国家自然科学基金-青年科学基金项目(31301466);北京市教委科技计划重点项目(KZ201410011015)

摘　　要：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。The analysis methods of the 3-methylthiopropanol in Sesame Flavor Liquor by Gas Chromatography-Mass Spectrum with Selected Ion Monitor（GC-MS/SIM） were established in this paper. The pretreatment method showed： the wine that concentrated 5 times was extracted by dichloromethane. The chromatographic method showed： the polar chromatographic column DB-FFAP（60 m × 0.25 mm × 0.25 μm）, programmed temperature. The condition of GC-MS were optimized, and the selected ions were m/z 106 and 61. External standard method was used in quantification. The analysis results showed： the linear behavior（R2= 0.9991） is very good under the concentration of 50 μg/L^10 mg/L, the LOD was5 μg/L, the LOQ was 10 μg/L, the recovery rate was between 83.8%~114.1% under the level of 80 μg/L, 800 μg/L and8 mg/L, the precision of within-day and inter-days were all less than 5%. Five brands and 21 samples were inspected.The 3-methylthiopropanol couldn＇t be detected in original or commercial wines of brand 1 and 3. It couldn＇t be detected in original wines of brand 2, while the concentration in the commercial wines of S-2-1, S-2-2, S-2-3 and S-2-4 were1.4, 0.36, 1.0, 0.66 mg/L, respectively. It couldn＇t be detected in commercial wines of brand 4, while the concentration in original wines of Y-4 was 2.4 μg/L. It couldn＇t be detected in original wines of brand 5, while the concentration in the commercial wines of S-5 was 0.24 mg/L.

关 键 词：3-甲硫基丙醇 自动质谱解卷积定性系统 相对丰度比 气相色谱-质谱/选择离子扫描法 芝麻香型白酒 

分 类 号：O657[理学—分析化学] TS262.3[理学—化学]