顶空液液萃取-气相色谱-质谱法用于白术挥发性成分的分析  

Analysis of Volatile Components of Atractylodes Macrocephala Koidz by Headspace Liquid Phase-Liquid-Phase Extraction Coupled with Gas Chromatography-Mass Spectrometry

作　　者：刘文涵[1] 何晶晶[1] 滕渊洁[1] 

机构地区：[1]浙江工业大学化学工程与材料学院,杭州310032

出　　处：《分析化学》2013年第8期1226-1231,共6页Chinese Journal of Analytical Chemistry

基　　金：浙江省分析测试基金(No.2012C37014);浙江省重点科技创新团队(No.2011R09002-12)资助

摘　　要：采用高温顶空液相萃取再转移的方法,对中药白术中挥发性成分进行萃取分离富集,采用顶空液液萃取/气相色谱-质谱(HS-LP-LPE/GC-MS)联用法进行测定,并与传统水蒸汽蒸馏法(SD)提取的挥发性成分进行对比。对各种测定条件和影响因素进行了考察,最佳萃取条件为:1.0 mL PEG 400为高温萃取剂,样品用量1.2 g,萃取温度120℃,萃取时间60 min,再将萃取剂用1.0 mL正己烷进行反萃取后进行GC-MS分析;采用HS-LP-LPE/GC-MS鉴定了33个组分,占总组分含量93.18%;SD鉴定了31个组分,占总组分含量97.12%。两种方法共同检测到的组分有29个,均以苍术酮(Atractylone)含量最高。结果表明,两种方法所提取的组分基本相同,可用于白术挥发性成分的测定。A novel headspace liquid phase-liquid-phase extraction coupled with gas chromatography-mass spectrometry（HS-LP-LPE/GC-MS） was developed by headspace liquid-phase extraction under high temperature to separate and enrich volatile components in Atractylodes macrocephala Koidz,which was then compared with traditional steam distillation（SD）.The variable experimental conditions were optimized,using 1.0 mL PEG 400,1.2 g sample,120 ℃ extraction temperature and 60 min extraction time.PEG 400 was then back extracted by 1.0 mL hexane for GS-MS.33 components accounting for 93.18% were identified by HS-LP-LPE/GC-MS,and 31 components accounting for 97.12% were identified by SD.29 common components were all identified and the Atractylone was the highest in both two methods,which shows that HS-LP-LPE/GC-MS can be used for determination of volatile components in Atractylodes macrocephala Koidz.

关 键 词：顶空液液萃取 气相色谱-质谱 挥发性成分 白术 分离富集 

分 类 号：R284[医药卫生—中药学]