色谱

色谱 ›› 2013, Vol. 31 ›› Issue (3): 240-248.DOI: 10.3724/SP.J.1123.2012.10031

• 研究论文 • 上一篇    下一篇

微波-超声波协同一步提取衍生化-气相色谱-质谱联用快速分析中药材猫爪草中的脂肪酸

詹汉英, 刘瑞林, 王德金, 袁静, 胥生杰, 张志琪*   

  1. 药用资源与天然药物化学教育部重点实验室, 陕西师范大学化学化工学院, 陕西 西安 710100
  • 收稿日期:2012-11-05 修回日期:2012-12-12 出版日期:2013-03-28 发布日期:2013-03-22
  • 通讯作者: 张志琪
  • 基金资助:

    国家自然科学基金项目(21275098).

Rapid determination of fatty acids in Ranunculus ternatus Thunb. by microwave-ultrasonic synergistic one-step extraction-derivatization and gas chromatography-mass spectrometry

ZHAN Hanying, LIU Ruilin, WANG Dejin, YUAN Jing, XU Shengjie, ZHANG Zhiqi*   

  1. Key Laboratory of Medicinal Resource and Natural Pharmaceutical Chemistry of Ministry of Education, School of Chemistry and Chemical Engineering, Shaanxi Normal University, Xi’an 710100, China
  • Received:2012-11-05 Revised:2012-12-12 Online:2013-03-28 Published:2013-03-22
  • Contact: Zhi-Qi ZHANG

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511

被引次数

17

摘要： 建立了一种微波-超声波协同一步提取衍生化、气相色谱-质谱联用快速测定中药材猫爪草中低含量脂肪酸的方法。以总脂肪酸的色谱峰面积为响应指标,采用响应曲面法优化了主要工艺参数,其结果为: 猫爪草粉末5.0 g,正己烷50.0 mL,微波功率500 W,反应温度50 ℃,催化剂用量0.30 g,甲醇用量4.0 mL,提取衍生化时间8 min。以内标法定量各个脂肪酸的含量,一步提取衍生化法获得的总脂肪酸峰面积((3.327±0.023)×107, n=3)和总不饱和脂肪酸含量((13.59±0.30) mg/g, n=3)明显高于传统方法((2.410±0.036)×107(n=3)和(12.05±0.34) mg/g(n=3))。该方法简化了复杂的样品处理过程,缩短了反应时间,降低了分析成本,改善了提取和衍生化效率,尤其是减少了不饱和脂肪酸的氧化和分解。该方法具有简单、快速和实用性的特点,是一种极具应用潜力的中药材中低含量脂肪酸的快速分析方法。

关键词: 猫爪草, 气相色谱-质谱联用, 微波-超声波协同作用, 响应曲面优化法, 一步提取衍生化, 脂肪酸

Abstract: A rapid and simple microwave-ultrasonic synergistic one-step extraction-derivatization (MUED) method and gas chromatography-mass spectrometry was established for the determination of low content fatty acids (FAs) profile in Ranunculus ternatus Thunb. The critical experimental parameters for MUED method were optimized with response surface methodology by taking the chromatographic peak areas of total FAs as a major response index. The best technological parameters were determined as 5.0 g of Ranunculus ternatus Thunb. powder, 50.0 mL of n-hexane, 500 W of microwave power, 50 ℃ of reaction temperature, 0.30 g of catalyst (KOH), 4.0 mL of derivatization reagent (methanol) and the time of extraction-derivatization of 8 min. The contents of individual FAs were quantified by internal standard method. The results showed that the chromatographic peak areas of the total FAs and the total unsaturated FAs contents obtained with MUED were (3.327±0.023)×107 (n=3) and (13.59±0.30) mg/g (n=3) respectively. They were markedly higher than those obtained by the conventional method which were (2.410±0.036)×107 (n=3) and (12.05±0.34) mg/g (n=3) respectively. The MUED method simplified the complicated sample handling steps, shortened the sample preparation time, reduced the cost of analysis, and improved the extraction and derivatization efficiency of the lipids, especially weakened the oxidization and decomposition of the unsaturated FAs. The simplicity, speed and practicability suggest the proposed method has significant potential for the determination of low content FAs in herbal medicines.

Key words: fatty acids, gas chromatography-mass spectrometry (GC-MS), microwave-ultrasonic synergistic action, Ranunculus ternatus Thunb., response surface methodology, one-step extraction-derivatization

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