Microwave-assisted one-step extraction-derivatization for rapid analysis of fatty acids profile in herbal medicine by gas chromatography-mass spectrometry.
Microwave-assisted one-step extraction-derivatization for rapid analysis of fatty acids profile in herbal medicine by gas chromatography-mass spectrometry.
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DOI：
10.1039/c2an36178g
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发表时间：
2012-10
期刊：
影响因子：
--
通讯作者：
Rui-Lin Liu;Jing Zhang;Zhao-li Mou;Shuang Hao;Zhiqi Zhang
中科院分区：
文献类型：
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作者：
Rui-Lin Liu;Jing Zhang;Zhao-li Mou;Shuang Hao;Zhiqi Zhang
建立了一种快速、实用的微波辅助一步萃取-衍生化气相色谱-质谱分析中草药中脂肪酸的方法。采用响应面法对微波辅助电子衍射的反应温度、微波功率和衍生试剂甲醇用量等关键实验参数进行了优化。结果表明，微波辅助提取法测得的总脂肪酸和总不饱和脂肪酸的色谱峰面积明显高于传统索氏提取法和微波提取衍生法。衍生反应的动力学和热力学研究表明，微波辅助可以降低衍生反应的活化能，增加阿累尼乌斯指前因子。MAED法简化了样品前处理程序，缩短了反应时间，提高了脂类的萃取和衍生效率，减少了成分损失，尤其是不饱和脂肪酸的氧化和异构化。该方法简单、快速、实用，为天然药物样品中脂肪酸的高通量分析提供了一种新的方法。
A rapid and practical microwave-assisted one-step extraction-derivatization (MAED) method was developed for gas chromatography-mass spectrometry analysis of fatty acids profile in herbal medicine. Several critical experimental parameters for MAED, including reaction temperature, microwave power and the amount of derivatization reagent (methanol), were optimized with response surface methodology. The results showed that the chromatographic peak areas of total fatty acids and total unsaturated fatty acids content obtained with MAED were markedly higher than those obtained by the conventional Soxhlet or microwave extraction and then derivatization method. The investigation of kinetics and thermodynamics of the derivatization reaction revealed that microwave assistance could reduce activation energy and increase the Arrhenius pre-exponential factor. The MAED method simplified the sample preparation procedure, shortened the reaction time, but improved the extraction and derivatization efficiency of lipids and reduced ingredient losses, especially for the oxidization and isomerization of unsaturated fatty acids. The simplicity, speed and practicality of this method indicates great potential for high throughput analysis of fatty acids in natural medicinal samples.