医学研究与教育 ›› 2025, Vol. 42 ›› Issue (2): 25-36.DOI: 10.3969/j.issn.1674-490X.2025.02.003

• 中医药学 • 上一篇    

基于方剂学和液-质联用方法的武当道墨质量分析研究

凌旭1,2,戢太阳3,金永昌2,金志雄2   

  1. 1.湖北医药学院药学院药物质检教研室, 湖北 十堰 442000;
    2.武当特色中药研究湖北省重点实验室, 湖北 十堰 442000;
    3.湖北医药学院附属东风总医院药学部, 湖北 十堰 442001
  • 收稿日期:2024-10-12 发布日期:2025-05-23
  • 通讯作者: 金志雄(1967—),男,湖北郧县人,教授,博士,主要从事微生物应用研究。E-mail: jzx8801150@sina.com
  • 作者简介:凌旭(1990—),男,湖北郧西人,讲师,博士,主要从事中药分析相关研究。 E-mail: 1300930550@qq.com
  • 基金资助:
    湖北医药学院博士科研启动金(k1276501);湖北省优势特色学科群项目基金(2021-2025)(2022BMXKQT2);湖北医药学院大学生创新创业训练项目(X202313249004);湖北医药学院武当道墨专项项目

  • Received:2024-10-12 Published:2025-05-23

摘要: 目的 发展武当道墨的快速简便分析方法,用于综合评价武当道墨的质量。方法 查阅中国药典结合方剂学对武当道墨处方进行分析。采用容量分析法测定其物理常数和化学成分含量。基于回流提取法提取制剂中极性较大易溶出组分并采用高效液相色谱-质谱联用技术(High Performance Liquid Chromatography-Mass Spectrometry,HPLC-MS)对其进行鉴别和测定。结果 武当道墨性温、寒,味辛、苦,主要归于肝经、心经,主升、浮,主功效为消肿解毒、排脓止痛。其密度为1.416 g/cm3,熔程为47~77 ℃,pH值为8.03.挥发油含量约为0.04 mL/g,其中阿魏酸、丹皮酚、金合欢素、乌头碱、士的宁等5个成分含量最高。毒性生物碱含量限度符合国家标准。 结论 本研究初步探明了武当道墨处方性味归经、功效和主要成分,阐释了成分与药理药效之间的关系,为建立其质量分析方法提供了思路。

关键词: 武当道墨, 提取分离, 理化常数, 含量测定, 质量控制

Abstract: Objective To examine the physicochemical properties and principal components and develop a quick and simple quality control method for comprehensively evaluating the quality of Wudang Taoist ink and improving its quality stability. Methods By consulting the 2020 edition of Chinese Pharmacopoeia and analyzing the prescription of Wudang Taoist ink combined with the knowledge of traditional Chinese medicine formulae. At the same time, the physical constants, total polysaccharides, total flavonoids and volatile oil contents of Wudang Taoist ink were determined by physical method and titration analysis. The solvent type, extraction time, extraction times and extraction temperature were investigated and selected to extract and separate the polar and soluble components in Wudang Taoist ink. The soluble components were identified by HPLC method combined with HPLC-MS in MRM mode of mass spectrum, several peaks with large peak area were identified. Finally, four kinds of alkaloids, neoaconitine, aconitine, hypaconitine and strychnine were determined by HPLC method. Results The 42 medicinal herbs in Wudang Taoist ink prescription were mainly based on their warm, cold nature and their pungent, bitter taste. The main meridians were Ganjing and Xinjing, mainly ascending, floating. There were 11 flavors of toxic herbs. The main effects were the swelling detoxification, drainaging of pus to relieve pain, clearing heat and blood circulation to remove blood stasis. The physical and chemical analysis results showed that Wudang Taoist ink had soft texture, with a density of 1.416 g/cm3, and the melting range of 47-77 ℃, the acidity value of 8.03. The contents of polysaccharide and volatile oil were 61.75 μg/g and 0.04 mL/mg. The optimized extraction solvent was methanol-water(1∶1, v/v), the extraction time was 30 min, the extraction times was once, and the extraction temperature was 90℃. Under these conditions the extraction solution was prepared and blown dry with nitrogen and redissolved and then 20 μL was injected into HPLC. The results showed that 28 chromatographic peaks were detected, the ferulic acid, paeonol, acacia, monosinand and other components were confirmed to have the highest content. Conclusion The flavor, meridian tropism and positive components of Wudang Taoist ink are preliminarily found out, and the relationships between components and pharmacological effects are explained, which provides ideas for establishing quality analysis methods of Wudang Taoist ink.

Key words: Wudang Taoist ink, extraction and separation, physical and chemical constants, content determination, quality control

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