固相微萃取和同时蒸馏萃取与气相色谱/质谱法分析芥末膏制品的风味成分  

Analysis of Volatile Constituents of Mustard Paste by Gas Chromatography/Mass Spectrometry with Solid-Phase Microextraction and Simultaneous Distillatilation and Extraction

作　　者：刘百战[1] 

机构地区：[1]中国科学技术大学经济技术学院,合肥230052

出　　处：《分析化学》2000年第12期1489-1492,共4页Chinese Journal of Analytical Chemistry

摘　　要：采用固相微萃取和同时蒸馏萃取技术分离芥末膏制品的挥发性成分，用ＧＣ／ＭＳ分析鉴定，对总离子流色谱的峰面积进行归一化定量。共鉴定了２２种化学成分，占总峰面积的９９％以上，其中含硫化合物８种，含氮化物３种，含氧化合物１１种。最主要的成分是异硫氰酸烯丙酯，其次是丙二醇，其他主要成分还有对羟基二叔丁基甲苯、油酸、９－十六烯酸、棕榈酸、５－甲基四氢噻吩－２－酮、二烯丙基二硫化物、异硫氰酸苯乙酯等。比较了各种萃取技术对分析结果的影响，同时蒸馏萃取法不能分离出水溶性成分如丙二醇等，在固相微萃取方法中，聚二甲基硅氧烷纤维头对极性较强的成分的取样效果不理想，聚乙二醇－二乙烯苯纤维头顶空取样的萃取效果最好。The voltile constituents of mused paste were investigated by solid-phase nicroextraction (SPME) and simultaneous distillation and extraction (SDE) and gas chromatography/mass spectrometry. In SPME experiments, 100 μm PDMS and 65 μm CW-DVB fibers were used. 4 .750 g of paste was added into 20 mL vial, heated at 70℃ for 60 min, then SPME fiber was inserted into the headspace of mustard paste, sampling at 70℃ for 30 min, the fiber was desorbed in gas chromatogrphic injection liner at 250℃ for 3 min with splitless mode. In SDE experiment, volatiles of 7. 135 g mustard paste were extracted into 30 mL dichloromethane, the extract was concentrated to 1. 0 mL, the injection volume was 2 .0 μL with a split ratio of 20: 1. A sulpecol-wax capillary colunm (30 m x 0. 25 mm i. d. + 0. 25 μm df) was employed to resolve the volatiles with following conditions: initial oven temperature 60℃, kept for 2 min, then raised to 240℃ 4℃/min, and dept at 240℃ for 15 min. Helium was used as carrier gas with column head pressure at 689 kPa. 22 volatile compounds were identified, the most predominant compound was allyl isothiocyanate, following it is propylene glycol, diallyl disulfide, BHT, 5-methyl tetrahydrothiophen-2-one, 2 - phenylethyl isothiocyanate, palmitic acid, 6- hexadecenoic acid and oleic acid, etc. Results obtained from different extiaction technique were also compared, SPME with 65 μm CW-DVB fiber gave the most desirable results.

关 键 词：芥末膏 风味成分分析 气相色谱-质谱法 

分 类 号：O657.7[理学—分析化学]