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| 咳喘浸手浴足I号挥发性成分的顶空-气相色谱-质谱分析 |
| 金实1,2,肖锋1,2,胡晓雪1,2,段雪云1,2,熊义涛1,2,王金波1,2,李成银1,2,孙婉瑾1,2 |
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| (1. 湖北省中医院,湖北武汉 430061;2. 湖北省中医药研究院,湖北武汉 430074) |
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| 摘要: |
| 目的：分析咳喘浸手浴足I号挥发性成分，为该中药复方制剂的进一步研究提供科学依据。方法：应用顶空静态加热萃取技术提取咳喘浸手浴足I号挥发性成分，采用顶空-气相色谱-质谱（HS-GC-MS）联用技术分析，使用Agilent DB-5MS毛细管色谱柱（0.25 μm×0.25 mm×30 m）分离，程序升温条件为初始温度40 ℃，保持3 min，以4 ℃/min升至120 ℃，保持5 min，以8 ℃/min升至160 ℃，保持5 min；载气为高纯氦气（纯度≥99.999%），载气流量 1.0 mL/min；分流比100:1，进样口温度200 ℃，进样量1 µL；质谱条件：电离方式EI，轰击电压70eV，正离子模式，离子源温度230 ℃。结果：从10批样品得到的HS-GC-MS图谱中共识别17个共有峰，结合文献识别为2,3,5,6-四甲基吡嗪（No.12，含量3.34%）、D-柠檬烯（No.8，含量16.26%）和α-蒎烯（No.3，含量6.94%）等相关物质。结论：本研究揭示了咳喘浸手浴足I号挥发性成分的组成情况，其中可能主要有效成分为2,3,5,6-四甲基吡嗪、D-柠檬烯和α-蒎烯，同时含有月桂烯、β-蒎烯、蒈烯等萜类透皮吸收促渗剂。 |
| 关键词: 顶空-气质-质谱联用技术 挥发性成分 咳喘浸手浴足I号 2,3,5,6-四甲基吡嗪 |
| DOI：10.13407/j.cnki.jpp.1672-108X.2021.01.001 |
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| 基金项目:基金项目:中国中医科学研究院中医基础研究所2018年院所协同创新科研专项基金,编号YZ-1850。 |
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| Headspace Sampling-Gas Chromatography-Mass Spectrometry Analysis of Volatile Components of Kechuan Jinshou Yuzu Powder I |
| Jin Shi1,2 , Xiao Feng1,2 , Hu Xiaoxue1,2 , Duan Xueyun1,2 , Xiong Yitao1,2 , Wang Jinbo1,2 , Li Chengyin1,2 , Sun Wanjin1,2 |
| (1. Hubei Provincial Hospital of Traditional Chinese Medicine, Hubei Wuhan 430061, China; 2. Hubei Academy of Traditional Chinese Medicine, Hubei Wuhan 430074, China) |
| Abstract: |
| Objective: To analyze the volatile components of Kechuan Jinshou Yuzu powder I, so as to provide reference for further study of traditional Chinese medicine compound preparation. Methods: Volatile components of Kechuan Jinshou Yuzu powder I were extracted by using headspace static heating extraction technology. Headspace sampling-gas chromatography-mass spectrometry (HS-GC-MS) technology was used for analysis. Agilent DB-5MS capillary column (0.25 m×0.25 mm×30 m) was used for separation. The programmed temperature was set as the initial temperature of 40 ℃, which was maintained for 3 min, then increased to 120 ℃ at 4 ℃/min, maintained for 5 min, and increased to 160 ℃ at 8 ℃/min, maintained for 5 min. The carrier gas was high-purity helium (purity ≥99.999%), with the carrier gas flow rate of 1.0 mL/min. The splitting ratio was 100∶1, inlet temperature was 200℃ and injection volume was 1µL. Mass spectrometry conditions: ionization mode EI, bombardment voltage 70eV, positive ion mode, ion source temperature 230 ℃. Results: The HS-GC-MS map obtained from 10 samples identified 17 common peaks, including 2,3,5,6-tetraminepyrazine (No.12, 3.34%), D-limonene (No.8, 16.26%), α-pinene (No.3, 6.94%) and other related substances. Conclusion: This study reveals the composition of volatile components of Kechuan Jinshou Yuzu powder I, among which the main effective components may be 2,3,5,6-tetramethylpyrazine, D-limonene and α-pinene, as well as transdermal absorption enhancers including myrcene, β-pinene and carene. |
| Key words: headspace sampling-gas chromatography-mass spectrometry technology volatile components Kechuan Jinshou Yuzu powder I 2,3,5,6-tetramethypyrazine |
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