| 王小宁,董馨,布仁,王跃武,于娟,陆景坤.通过量效关系评价CO2超临界提取肉豆蔻挥发油质量[J].中国药事,2024,38(9):1020-1031 |
| 通过量效关系评价CO2超临界提取肉豆蔻挥发油质量 |
| Evaluating the Quality of Volatile Oil Extracted from Nutmeg by CO2 Supercritical Extraction by Dose-effect Relationship |
| 投稿时间：2024-06-05 |
| DOI：10.16153/j.1002-7777.20240457 |
| 中文关键词: 肉豆蔻挥发油 CO2超临界萃取法 气相色谱-三重四极杆质谱 含量测定 量效关系 |
| 英文关键词: volatile oil of nutmeg CO2 supercritical extraction method GC-MS/MS content determination dose-eff ect relationship |
| 基金项目:国家自然科学基金（编号 82260813，81960757）；内蒙古自然科学基金（编号 2020MS08045）；内蒙古医科大学重点项目（编号 YKD2023ZD005） |
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| 中文摘要: |
| 目的：气相色谱-三重四极杆质谱（GC-MS/MS）法定量分析16批次肉豆蔻挥发油中4-萜烯醇、 α-蒎烯、甲基丁香酚、榄香素、黄樟素和肉豆蔻醚，结合抗炎活性量效分析，对肉豆蔻的药效成分进行质量评价。方法：采用CO2超临界萃取法提取肉豆蔻挥发油，建立GC-MS/MS法分析肉豆蔻中6个成分的检测方法，进行方法学考察并对16批次挥发油样品中6个成分进行含量测定。气相色谱条件：J&W DB-17ms气相色谱柱（30 m×0.25 mm，0.25 μm）；升温程序：50 ℃，保持1 min，以10 ℃·min-1的速率升高到150 ℃，保持3 min；再以20 ℃·min-1的速率升高到250 ℃，保持3 min。进样口温度280 ℃； 载气为氮气，流速为1 mL·min-1，分流比为10∶1，进样量为1 μL；建立16批次挥发油处理脂多糖 （LPS）诱导的Raw264.7巨噬细胞炎症模型，并进行药效分析；对挥发油中6个成分进行主成分分析 （PCA-X）、Pearson相关性分析及药效分析，并将变量重要性投影（VIP）值＞1及Pearson系数为正的化合物作为贡献性成分。结果：4-萜烯醇、α-蒎烯、甲基丁香酚、榄香素、黄樟素、肉豆蔻醚在相应的浓度范围内呈现良好的线性关系；6个成分精密度试验的RSD在0.18%~0.90%，重复性试验的RSD在 1.53%~2.90%，稳定性试验的RSD在2.11%~2.94%；平均加样回收率（n=9）分别为98.32%、99.41%、 94.79%、98.82%、96.14%、97.81%，RSD分别为1.51%、1.62%、1.87%、0.71%、1.82%、1.31%。16 批次挥发油样品中4-萜烯醇、α-蒎烯、甲基丁香酚、榄香素、黄樟素、肉豆蔻醚的含量范围分别为 4.674~12.432、2.316~11.121、0.201~4.653、1.047~10.488、201.776~402.163、7.888~39.570 mg·g-1。 量效关系分析显示，抗炎活性与6个成分含量具有一定的相关性，甲基丁香酚、榄香素、肉豆蔻醚对抗炎活性有贡献，其中榄香素贡献最大。结论：建立了肉豆蔻16批次挥发油中6个成分的抗炎活性量效关系分析方法，本法简便快速，为肉豆蔻的质量控制及安全、有效的应用提供依据。 |
| 英文摘要: |
| Objective: Gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) was used to quantitatively analyze terpinen-4-ol, α-pinene, methyleugenol, elemicin, safrole and myristcin in 16 batches of volatile oil of nutmeg. Combined with anti-inflammatory activity dose-effect analysis, the quality of the active ingredients in nutmeg was evaluated. Methods: CO2 supercritical extraction method was used to extract the volatile oil of nutmeg, and a GC-MS/MS method was established to analyze the six components in nutmeg. Methodological investigation was conducted and the content of six components in 16 batches of volatile oil samples was determined. Gas chromatographic conditions: J&W DB-17ms gas column (30 m×0.25 mm, 0.25 μm); temperature rise procedure: 50 ℃, keep for 1 min, rise to 150 ℃ at the rate of 10 ℃·min-1, keep for 3 min; then it was raised to 250 ℃ at the rate of 20 ℃·min-1 and keep for 3 min. Inlet temperature 280 ℃; the carrier gas was nitrogen, the flow rate was 1 mL·min-1, the shunt ratio was 10∶1, and the sample size was 1 μL. The inflammation model of Raw264.7 macrophages induced by lipopolysaccharide (LPS) was established in 16 batches of volatile oil, and the pharmacodynamic analysis was performed. The volatile oil samples were analyzed by principal component analysis (PCA-X) and Pearson coefficient was positive compounds as contributing components. Results: There was a good linear relationship between terpinen-4-ol, α-pinene, methyleugenol, elemicin, safrole and myristicin in the corresponding concentration range. RSD of the six components ranged from 0.18% to 0.90% for precision test, 1.53% to 2.90% for repeatability test, and 2.11%-2.94% for stability test. The average recoveries (n=9) were 98.32%, 99.41%, 94.79%, 98.82%, 96.14%, 97.81%, and RSD was 1.51%, 1.62%, 1.87%, 0.71%, 1.82%, 1.31%, respectively. The contents of terpinen-4-ol, α-pinene, methyleugenol, elemicin, safrole and myristicin in 16 batches of volatile oil samples ranged from 4.674-12.432 mg·g-1, 2.316-11.121 mg·g-1, 0.201-4.653 mg·g-1, 1.047-10.488 mg·g-1, 201.776-402.163 mg·g-1, 7.888-39.570 mg·g-1, respectively. The results showed that there was a correlation between the anti-inflammatory activity and the content of six components. The anti-inflammatory activity of methyleugenol, elemicin and myristicin contributed, and elemicin contributed the most. Conclusion: A dose-effect relationship analysis was established for the anti-inflammatory activity of six components in 16 batches of volatile oil of nutmeg. The method is simple and rapid, and provides a basis for the quality control, safe and effective application of nutmeg. |
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