固相微萃取、液液萃取结合气相色谱-质谱法分析芝麻香型白酒中的含硫化合物

应用固相微萃取法、液液萃取法结合气相色谱-质谱联用分析手段对芝麻香型白酒中含硫化合物进行定性分析。通过配制模拟酒样对固相微萃取法、液液萃取法的前处理条件进行优化。在最优条件下对36 个芝麻香型白酒酒样中的微量成分提取分析，固相微萃取法共检出178 种挥发性成分，液液萃取法共检出239 种挥发性成分。两种方法共检出14 种含硫化合物，均采用标准品比对进行准确定性。首次在中国白酒中检测出硫代丁酸甲酯、糠基甲基硫醚、硫代呋喃甲酸甲酯、4-甲基二苯并噻吩、3-甲硫基丁醛、甲基硫代磺酸甲酯6 种含硫化合物；此外，首次在芝麻香型白酒中检出苯并噻唑和苯并噻吩。

Analysis of Sulfur-Containing Compounds in Sesame-flavor Chinese Liquor by Solid Phase Microextraction and Liquid-Liquid Extraction Coupled with GC-MS

The sulfur-containing compounds of sesame-flavor Chinese liquor were analyzed by solid phase microextraction (SPME) and liquid-liquid extraction (LLE) coupled with gas chromatography-mass spectrometry (GC-MS). Using a simulated liquor sample, the optimum experimental conditions were determined. A total of 178 volatiles were identified by SPME combined with GC-MS and 239 volatiles by LLE combined with GC-MS. Among them, 14 sulfur-containing compounds were identified by comparing mass spectra and linear retention indices (RI) of those of standards in 36 sesame-flavor Chinese liquor samples. S-Methyl ester butanethioic acid, 2-(methylthio)methyl]-furan, S-methyl ester 2-furancarbothioic acid, 4-methyl-dibenzothiophene, 3-methylthiobutyraldehyde, and S-methyl methanethiosulphonate were detected in Chinese liquor for the first time; In addition, benzothiazole and benzo b] thiophene were detected in sesame-flavor Chinese Baijiu for the first time.