溶剂法提取分蘖葱头有机硫化合物及其GC-MS分析

摘要

为研究有机溶剂对分蘖葱头中有机硫化合物提取及成分的影响,采用二氯甲烷、乙酸乙酯、正己烷3种溶剂提取分蘖葱头中有机硫化合物,并利用顶空固相微萃取和气相色谱-质谱联用技术对不同溶剂提取到有机硫化合物进行比较分析.结果表明:二氯甲烷提取分蘖葱头中有机硫化合物的最佳工艺条件为浸提时间4h、料液比1∶4(g/mL)、搅拌速率250 r/min,在此条件下有机硫化合物得率为(0.413 3±0.007)％.乙酸乙酯、正己烷有机硫化合物得率分别为(0.273 3±0.011)％、(0.288 9±0.009)％.3种溶剂共提取分离出45种组分,均检测出9种有机硫化合物,其中相对含量较高的均为噻吩类和硫醚类.另外,以二氯甲烷为溶剂提取出独有的有机硫化合物12种;以乙酸乙酯为溶剂提取出独有的有机硫化合物3种;以正己烷为溶剂提取出独有的有机硫化合物8种.%In this study,we examined the effects of different organic solvents on the extraction efficiency and composition of organic sulfur-containing compounds from tillering onion.The organic sulfur-containing compounds were extracted by dichloromethane and ethyl acetate and n-hexane,respectively,and then analyzed by headspace solid phase microextraction and gas chromatography-mass spectrometry (HS-SPME-GC-MS).The optimum extraction conditions with dichloromethane as the extraction solvent were determined to be 4 h extraction at a ratio of material to liquid of 1:4 (g/mL) with stirring at 250 r/min,leading to a yield of (0.413 3 ± 0.007)％,which was higher than those obtained with ethyl acetate and n-hexane as the extraction solvent,(0.273 3 ± 0.011)％ and (0.288 9 ± 0.009)％,respectively.A total of 45 components were extracted by the three solvents and 9 organic sulfur-containing compounds were detected in each solvent extract,among which,thiophenes and thioethers were predominant.In addition,12,3 and 8 unique organic sulfur-containing compounds were extracted by methylene chloride,ethyl acetate,and n-hexane.