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  

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

作　　者：赵东瑞[1] 张丽末 张锋国 孙金沅[1,3] 孙啸涛[1,3] 黄明泉[1,3] 郑福平[1,3] 孙宝国[1,3] ZHAO Dongrui ZHANG Limo ZHANG Fengguo SUN Jinyuan SUN Xiaotao HUANG Mingquan ZHENG Fuping SUN Baoguo(Beijing Key Laboratory of Flavor Chemistry, Beijing Technology and Business University, Beijing 100048, China Beijing Advanced Innovation Center for Food Nutrition and Human Health, Beijing Technology and Business University, Beijing 100048, China Technology Center of Guojing Co. Ltd., Gaoqing 256300, China)

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]山东国井集团技术中心,山东高青256300 [3]北京工商大学北京食品营养与人类健康高精尖创新中心,北京100048

出　　处：《食品科学》2016年第22期99-106,共8页Food Science

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：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。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 sesameflavor Chinese Baijiu for the first time.

关 键 词：固相微萃取法 液液萃取法 气相色谱-质谱 芝麻香型白酒 含硫化合物 

分 类 号：TS207.3[轻工技术与工程—食品科学]