色谱

色谱 ›› 2012, Vol. 30 ›› Issue (05): 515-521.DOI: 10.3724/SP.J.1123.2011.11024

• 研究论文 • 上一篇    下一篇

莪术中挥发性成分的微波辅助固相顶空气相色谱法分析

傅小红, 陈华*, 杨丰庆, 夏之宁   

  1. 重庆大学化学化工学院, 重庆 400044
  • 收稿日期:2011-11-14 修回日期:2011-12-21 出版日期:2012-05-28 发布日期:2012-06-07
  • 通讯作者: 陈华,副教授,研究方向为药物分析. Tel: (023)65106615, E-mail: chenhuacqu@yahoo.com.cn.
  • 基金资助:

    国家自然科学基金项目(21005092)、重庆市自然科学基金项目(2010BB0063)和中央高校基本科研业务费项目(11220004).

Analysis of volatile compounds from Curcuma by microwave assisted solid phase headspace-gas chromatography

FU Xiaohong, CHEN Hua*, YANG Fengqing, XIA Zhining   

  1. College of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400044, China
  • Received:2011-11-14 Revised:2011-12-21 Online:2012-05-28 Published:2012-06-07
  • Contact: Hua CHEN

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摘要： 将微波无溶剂提取(SFME)与顶空气相色谱(HS-GC)在线联用,建立了中药材的微波辅助固相顶空气相色谱法(MASP-HSGC),并用该方法快速直接分析了莪术药材中的挥发性成分。研究中对色谱条件、微波作用时间、微波作用功率等因素进行了考察,并以莪术醇为标准品考察了回收率和检出限,同时测定了莪术醇在莪术药材中的含量。对采用水蒸气蒸馏法(HD)和SFME法获得的莪术挥发油进行了气相色谱-质谱（GC-MS）分析,所得结果与所建立方法的结果进行对比。结果表明: HD-GC、SFME-GC和MASP-HSGC法所测得的化合物分别为35、33和40种;3种方法测得的莪术醇含量分别为（0.294±0.015）、（0.331±0.023）和（0.297±0.009） mg/g。该法简便快速,可用于莪术中挥发性成分的分离分析。

关键词: 顶空气相色谱法, 莪术, 固相, 挥发性成分, 微波无溶剂提取, 中药材

Abstract: A novel method of microwave assisted solid phase headspace gas chromatography (MASP-HSGC) was developed through online coupling of solvent-free microwave extraction (SFME) and headspace-gas chromatography via a six-way valve. The method can quickly and directly analyze the volatile compounds from solid samples with its ability of simultaneous extraction, separation and analysis without any pretreatment. The method was applied to analyze the volatile compounds of solid Curcuma. Some experimental parameters such as the chromatographic conditions, microwave power and irradiation time were studied. Curcumol was used as the standard to evaluate the recovery, the limit of detection and the contents of compounds in a Curcuma sample. The essential oils were prepared by hydrodistillation extraction (HD) and SFME separately, and analyzed by gas chromatography-mass spectrometry (GC-MS) to compare the results with those from the developed method. It showed that the numbers of compounds obtained by the three methods of HD-GC, SFME-GC and MASP-HSGC were 35, 33, 40 respectively. The contents of curcumol using the three methods were (0.294±0.015), (0.331±0.023), (0.297±0.009) mg/g respectively. The method was approved to be suitable for the rapid analysis of volatile components in Curcuma.

Key words: Chinese medical material, Curcuma, headspace-gas chromatography (HS-GC), solid phase, volatile compounds, solvent-free microwave extraction (SFME)

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