川芎挥发油的GC-MS定性分析及丁烯基苯酞和藁本内酯的含量测定

doi:10.5246/jcps.2021.05.034

中国药学(英文版) ›› 2021, Vol. 30 ›› Issue (5): 434-445.DOI: 10.5246/jcps.2021.05.034

川芎挥发油的GC-MS定性分析及丁烯基苯酞和藁本内酯的含量测定

闫玺镁, 高太祥, 石莉尧, 王瑞^*()

山西中医药大学中药与食品工程学院, 山西晋中 030619

收稿日期:2020-10-26 修回日期:2020-12-15 接受日期:2021-01-08 出版日期:2021-05-31 发布日期:2021-05-29
通讯作者: 王瑞
作者简介:
+ Tel.: +86-351-3179903, E-mail: wrgreentea@163.com
基金资助:
Shanxi pharmaceutical comprehensive development and utilization collaborative innovation center project (Grant No. 2017JYXT15), Science and technology innovation team project of Shanxi University of Traditional Chinese Medicine (Grant No. 2018TD-008) and "Basic research project" of Shanxi University of traditional Chinese Medicine (Grant No. 2020PY-JC-20).

Qualitation of Chuanxiong Rhizome essential oil and determination of 3-butylidenephthalide and ligustilide by GC-MS

Ximei Yan, Taixiang Gao, Liyao Shi, Rui Wang^*()

College of Pharmacy, Dalian Medical University, Dalian 116000, China

Received:2020-10-26 Revised:2020-12-15 Accepted:2021-01-08 Online:2021-05-31 Published:2021-05-29
Contact: Rui Wang

摘要/Abstract

摘要：

川芎是一种治疗心血管疾病的传统中药, 其主要活性成分为挥发油。本研究建立了一种基于SIM扫描模式和批处理分析的GC-MS定量方法, 并以丁烯基苯酞和藁本内酯的总含量为指标, 对水蒸气蒸馏法、超声提取法和CO2超临界萃取法三种挥发油提取方法进行工艺优化, 对三种方法所得挥发油进行成分鉴定和含量测定。结果表明, 3种方法提取的挥发油中, 超声提取所得丁烯基苯酞和藁本内酯的提取率最高, 水蒸气蒸馏法所得挥发油的化学成分种类最多, 超临界萃取法所得挥发油量最多, 得油率最高。

关键词: 川芎, 丁烯基苯酞, 藁本内酯, GC-MS, SIM扫描

Abstract:

Chuanxiong Rhizoma (rhizomes of Ligusticumchuanxiong Hort) is a classical Chinese medicine, and it is usually used for the treatment of cardiovascular diseases. The essential oil is the main active constituent of Chuanxiong. In this study, a GC-MS quantitative method based on the SIM scanning mode and batch processing analysis was established, and the total contents of 3-butylidenephthalide and ligustilide were used as the indicators to optimize three extraction methods, including hydro-distillation extraction (HDE), ultrasound-assisted extraction (UAE) and supercritical fluid extraction (SFE). Then the volatile oil obtained by three extraction methods was analyzed qualitatively. The results showed that the volatile oil obtained by the UAE had the highest contents of 3-butylidenephthalide and ligustilide, the volatile oil extracted by HDE had the most types of chemical components, and the SFE volatile oil had the highest oil yield.

Key words: Ligusticumchuanxiong Hort, 3-Butylidenephthalide, Ligustilide, GC-MS, SIM scanning

Supporting:

闫玺镁, 高太祥, 石莉尧, 王瑞. 川芎挥发油的GC-MS定性分析及丁烯基苯酞和藁本内酯的含量测定[J]. 中国药学(英文版), 2021, 30(5): 434-445.

Ximei Yan, Taixiang Gao, Liyao Shi, Rui Wang. Qualitation of Chuanxiong Rhizome essential oil and determination of 3-butylidenephthalide and ligustilide by GC-MS[J]. Journal of Chinese Pharmaceutical Sciences, 2021, 30(5): 434-445.

图/表 17

Table 1. SIM scanning mode.

Table 2. Factors and levels of orthogonal test.

Table 3. Results and analysis of the orthogonal test.

Table 4. Analysis of variance results.

Table 5. Factors and levels of the orthogonal test.

Table 6. Results and analysis of the orthogonal test.

Table 7. Analysis of variance results.

Table 8. Factors and levels of the orthogonal test.

Table 9. Results and analysis of the orthogonal test.

Table 10. Analysis of variance results.

Table 11. Three batches of verified content.

Figure 1. TIC with SIM scanning of 3-butylidenephthalide.

Figure 2. TIC with SIM scanning of ligustilide.

Figure 3. TIC with SIM scanning of essential oil by CO2-SFE (1. 3-Butylphthalide; 2. Ligustilide. Red is HDE; Green is UAE; Black is CO2-SFE).

Table 12. Method validation.

Table 13. The chemical composition of volatile oils.

Figure 4. TIC with full scanning of essential oil (Red is HDE; Green is UAE; Black is CO2-SFE).

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川芎挥发油的GC-MS定性分析及丁烯基苯酞和藁本内酯的含量测定

Qualitation of Chuanxiong Rhizome essential oil and determination of 3-butylidenephthalide and ligustilide by GC-MS

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