色谱

色谱

• 研究论文 • 上一篇    下一篇

顶空固相微萃取-气相色谱-质谱法用于白术中挥发性成分的分析

郭方遒1,黄兰芳1,2,周邵云1   

  1. 1.Research Center for Modernization of Chinese Herbal Medicine, College of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China; 2.Technical Center of Changde Cigarette Factory, Changde 415000, China
  • 收稿日期:2006-03-02 修回日期:2006-07-19 出版日期:2007-01-30 发布日期:1986-03-25
  • 通讯作者: 郭方遒

Headspace Solid-Phase Microextraction-Gas Chromatography-Mass Spectrometry for Analysis of Volatile Components from Atractlodes macrocephala Koidz.

GUO Fangqiu1, HUANG Lanfang1,2, ZHOU Shaoyun1   

  1. 1.Research Center for Modernization of Chinese Herbal Medicine, College of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China; 2.Technical Center of Changde Cigarette Factory, Changde 415000, China
  • Received:2006-03-02 Revised:2006-07-19 Online:2007-01-30 Published:1986-03-25
  • Contact: GUO Fangqiu

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1245

被引次数

130

摘要： 采用顶空固相微萃取-气相色谱-质谱法(HS-SPME-GC-MS)分离鉴定了白术中的挥发性成分,并与采用传统的水蒸气蒸馏法(SD)提取的挥发性成分进行了比较。实验中筛选了固相微萃取纤维头,优化了SPME的操作条件。样品在70 ℃下平衡30 min后，用65 μm聚二甲基硅氧烷-二乙烯基苯(PDMS-DVB)纤维头对白术样品顶空吸附30 min,于250 ℃下解吸4 min, 然后采用GC-MS对解吸物进行分离鉴定；采用HS-SPME-GC-MS鉴定出41种组分,占总峰面积的90.81%；采用SD-GC-MS鉴定出31个组分,占总峰面积的88.19%,且采用SD所提取的组分基本上都被固相微萃取所提取。结果表明, HS-SPME可取代耗时的SD用于白术中挥发性物质的提取。

关键词: 白术 , 顶空固相微萃取, 挥发性成分, 气相色谱-质谱, 水蒸气蒸馏

Abstract: Headspace solid-phase microextraction (HS-SPME) technique was employed to extract the volatile components from Chinese traditional medicine, Atractlodes macrocephala Koidz. The volatile components were isolated and identified successfully by gas chromatography-mass spectrometry(GC-MS). The results from HS-SPME-GC-MS were compared with those obtained from steam distillation-GC-MS (SD-GC-MS) with a good agreement. The volatiles were collected using a polydimethylsiloxane-divinylbenzene (PDMS-DVB) fiber by HS-SPME. The best response was obtained when the extraction temperature was 70 ℃, the equilibrium time and extraction time were all 30 min and the desorption time was 4 min. Analysis was performed by GC-MS with a polysiloxane capillary column (30 m×0.25 mm, film thickness 0.25 μm) using He as the carrier gas and a programmed temperature run. Forty-one components accounting for 90.81% were identified. The main components (relative amount more than 1%) of the samples by HS-SPME were atractylone (40.12%), γ-elemene (14.73%), aromadendrene (13.05%), eudesma-4(14),11-diene (5.46%), caryophyllene (2.56%), patchoulene (2.55%), 6,10,11,11-tetramethyl-tricyclo［6.3.0.1(2,3)］undec-7-ene (2.11%), cedrene (1.48%), α-caryophyllene (1.48%) and selina-4(14)-7(11)diene-8-one (1.01%). By SD-GC-MS, 31 components accounting for 88.19% were identified and all these components could be extracted by SPME except trans-β-ocimene which accounts only 0.10%. The results showed that the HS-SPME technique can be used to extract the the volatile components from Atractlodes macrocephala Koidz. in place of the traditional time-consuming SD.

Key words: Atractlodes macrocephala Koidz. , gas chromatography-mass spectrometry (GC-MS), steam distillation(SD), volatile components, head space solid-phase microextraction (HS-SPME)