Li Ning, Deng Chunhui, Li Yan, Ye Hao, Zhang Xiangmin
Department of Chemistry, Fudan University, Shanghai 200433, China.
J Chromatogr A. 2006 Nov 10;1133(1-2):29-34. doi: 10.1016/j.chroma.2006.08.046. Epub 2006 Sep 6.
In this paper, a novel method based on gas chromatography-mass spectrometry (GC-MS) following microwave distillation-headspace solid-phase microextraction (MD-HS-SPME) was developed for the determination of essential oil in dry traditional Chinese medicine (TCM). TCM is dried before being preserved and used, there is too little water to absorb microwave energy and heat the TCM samples. In the work, carbonyl iron powders (CIP) was added and mixed with the dried TCM sample, which was used as microwave absorption solid medium for dry distillation of the TCM. At the same time, SPME was used for the extraction and concentration of essential oil after MD. The dry rhizomes of Atractylodes lancea DC was used as the model TCM, and used in the study. The MD-HS-SPME parameters including fiber coating, microwave power, irradiation time, and the amount of added CIP, were studied. To demonstrate the method feasibility, the conventional HS-SPME method was also used for the analysis of essential oil in the TCM. Experimental results show that more compounds were isolated and identified by MD-HS-SPME than those by HS-SPME. Compared to conventional HS-SPME, the advantages of the proposed method are: short extraction time and high extraction efficiency. All experimental results show that the proposed method is an alternative tool for fast analysis of essential oils in dry TCMs.
本文开发了一种基于微波蒸馏-顶空固相微萃取（MD-HS-SPME）后气相色谱-质谱联用（GC-MS）的新方法，用于测定干燥中药中的挥发油。中药在保存和使用前需进行干燥处理，此时水分过少无法吸收微波能量并加热中药样品。在本研究中，添加羰基铁粉（CIP）并与干燥的中药样品混合，用作中药干馏的微波吸收固体介质。同时，采用固相微萃取（SPME）对微波蒸馏后的挥发油进行萃取和浓缩。以白术干燥根茎为模型中药进行研究。考察了纤维涂层、微波功率、辐照时间和羰基铁粉添加量等MD-HS-SPME参数。为验证该方法的可行性，还采用传统顶空固相微萃取（HS-SPME）法对中药中的挥发油进行分析。实验结果表明，与HS-SPME相比，MD-HS-SPME分离鉴定出的化合物更多。与传统HS-SPME相比，该方法具有萃取时间短、萃取效率高的优点。所有实验结果表明，该方法是快速分析干燥中药中挥发油的一种替代工具。
