【作者】 李晓霞；

【导师】 刘忠英；

【作者基本信息】 吉林大学 ， 药物分析学， 2021， 硕士

【摘要】 五味子(Schisandra chinensis(Turcz.)Baill)属木兰科植物,为吉林省道地药材。传统中医理论认为五味子用于入肺补肺,起到益气生津、收敛固涩的作用。临床常用的五味子炮制方法有蒸制、醋制、酒制、蜜制、盐制,而目前国家药典和吉林省炮制规范里五味子的炮制方法只有醋制。因此,为了满足临床需求和完善五味子炮制工艺规范与质量标准,本文将以五味子为研究对象,建立五味子木脂素含量测定方法,优选蒸五味子、盐五味子、蜜五味子最佳炮制工艺,建立相应质量标准,对五味子及其炮制品化学成分进行初步分析比较。为完善五味子质量标准和五味子药材进一步开发利用提供科学依据。主要研究内容包括以下几个方面:1.五味子木脂素含量测定方法研究建立一种测定五味子中8种木脂素含量的高效液相色谱法,对该方法进行条件优化和方法学验证。结果表明,该方法专属性强、准确度和精密度高、线性和稳定性好,可以用于五味子指标成分含量测定。2.蒸五味子、盐五味子、蜜五味子炮制工艺研究利用紫外-可见分光光度法和高效液相色谱法分别测定五味子总木脂素和8种木脂素成分的含量,并以木脂素为指标,对三种炮制工艺进行单因素实验、正交试验和验证实验。最终确定蒸五味子最佳炮制工艺为:取五味子药材10 g,加入10 m L清水拌匀,闷润1 h,置于蒸箱内蒸制3 h,取出,60℃烘干;盐五味子最佳炮制工艺:取五味子药材10 g,加入10 m L 1%盐水拌匀,闷润1 h,置于80℃炒锅内炒制60 s,取出,60℃烘干;蜜五味子最佳炮制工艺:取五味子药材10 g,加入10 m L 10%蜜水拌匀,闷润1 h,置于80℃炒锅内炒制60 s,取出,60℃烘干。3.五味子指纹图谱研究收集20批五味子药材,经检验均符合2020年版《中国药典》五味子标准各项规定。将每批分别制备成三种炮制品,采用高效液相色谱法,建立五味子及炮制品的指纹图谱,以中药色谱指纹图谱相似度评价系统进行分析,共标定11个共有峰,其8个共有峰有对照品指认。相似度分析结果表明20批药材样品及炮制品中的成分虽然一致,但含量差异较大。聚类分析结果与主成分分析结果基本一致,它们都将20批五味子分为3类,为完善质量标准奠定基础。4.五味子及其炮制品质量标准研究参考2020版《中国药典》五味子项下方法,分别考察20批五味子及其三种炮制品性状、鉴定项(薄层鉴别)、检查项(水分、灰分)及五味子炮制品中8种木脂素的含量。并在上述研究基础上,制定了五味子及其炮制品的质量标准(草案)。5.五味子炮制前后成分初步分析利用高效液相色谱法对五味子及其炮制品中5-羟甲基糠醛的含量进行测定并比较。相较与五味子,三种炮制品中5-羟甲基糠醛均有不同程度增加,且蒸五味子增加最多。采用GC-MS技术对五味子挥发油进行分析,结果表明三种炮制品中挥发油种类有所减少。综上所述,本文首先建立了一种测定8种五味子木脂素成分的高效液相色谱法。然后以木脂素为评价指标,考察蒸五味子、盐五味子、蜜五味子炮制工艺参数,确定各个炮制品的最佳炮制工艺。第三,基于指纹图谱技术结合相似度分析、聚类分析及主成分分析等方法,对五味子指纹图谱进行研究,为五味子药材及炮制品质量评价提供参考。最后,制定蒸五味子、盐五味子、蜜五味子的炮制规范和质量标准,对五味子及其三种炮制品中5-羟甲基糠醛、挥发油进行初步分析。为五味子及其炮制品规范生产、质量控制和临床应用提供了科学依据。更多还原

【Abstract】 Schisandra chinensis(Turcz.)Baill is a Magnoliaceae plant and is an authentic medicinal material in Jilin Province.Traditional Chinese medicine theory believes that Schisandra chinensis is used to enter the lungs and nourish the lungs,and play the role of nourishing qi,promoting body fluids,and astringent and astringent.The commonly used methods for preparing schisandra in clinical practice include steaming,vinegar,wine,honey,and salt.At present,the method of schisandra is only vinegar in the National Pharmacopoeia and Jilin Province.Therefore,in order to meet the clinical needs and improve the processing specifications and quality standards of schisandra,this article will take schisandra as the research object to establish a method for determining the content of schisandra lignans,and optimize the best processing technology for steamed schisandra,salt schisandra,and honey schisandra,and establish the corresponding quality Standard,preliminary analysis and comparison of the chemical composition of Schisandra and its processed products.Provide a scientific basis for improving the quality standards of schisandra and the further development and utilization of schisandra.The main research content includes the following aspects:1.Study on the determination method of Schisandra lignans contentA high performance liquid chromatography method for the determination of 8lignans in Schisandra chinensis was established,and the method was systematically investigated and verified by methodology.The results show that the method has strong specificity,high accuracy and precision,good linearity and stability,and can be used for the determination of schisandra index components.2.Research on the processing technology of steamed schisandra,salt schisandra and honey schisandraUsing single factor experiment and orthogonal experiment,UV-visible spectrophotometry and high performance liquid chromatography were used to determine the content of total lignans and 8 kinds of lignans in Schisandra chinensis,and lignans were used as an indicator to determine the content of three lignans.Orthogonal experiments and verification experiments were carried out for the processing technology.It is finally determined that the best processing technology for steamed schisandra is: take 10 g of schisandra medicinal material,add 10 m L of water and mix well,let it moisten for 1 h,steam it in a steamer for 3 h,take it out,and dry at60°C;salt schisandra is best processed Process: Take 10 g of Schisandra medicinal materials,add 10 m L of 1% salt water,mix well,moisten for 1 h,fry for 60 s in a wok at 80°C,take it out,and dry at 60°C;the best processing technology for honey schisandra: take schisandra 10 g of medicinal materials,add 10 m L of 10% honey water,mix well,moisten for 1 h,fry for 60 s in a wok at 80°C,take it out,and dry at60°C.3.Study on the fingerprint of Schisandra chinensis20 batches of Schisandra medicinal materials were collected,and all of them were in compliance with the requirements of the 2020 edition of the Chinese Pharmacopoeia standard for Schisandra.Each batch was prepared into three kinds of processed products,and the fingerprints of Schisandra and processed products were established by high performance liquid chromatography,and analyzed by the Chinese medicine chromatographic fingerprint similarity evaluation system.A total of 11 common peaks were calibrated,and 8 of them shared The peak is designated by the reference substance.The similarity analysis results show that although the ingredients in the 20 batches of medicinal material samples and processed products are the same,the contents are quite different.The cluster analysis results are basically the same as the principal component analysis results.They divided 20 batches of schisandra into 3categories.4.Study on the quality standards of Schisandra and its processed productsRefer to the methods under the schisandra item of the 2020 edition of the Chinese Pharmacopoeia to investigate the properties,identification items(thin layer identification),inspection items(moisture,ash)and 8 lignans in the schisandra processed products of 20 batches of schisandra and its three processed products Content.And on the basis of the above research,the quality standard(draft)of Schisandra and its processed products has been formulated.5.Preliminary analysis of schisandra before and after processingThe content of 5-hydroxymethyl furfural in Schisandra and its processed products was determined and compared by HPLC.Compared with schisandra,5-hydroxymethyl furfural in the three processed products increased to varying degrees,and steamed schisandra increased the most.Using GC-MS technology to analyze the volatile oil of Schisandra,the results show that the types of volatile oil in the three processed products have been reduced.In summary,this article first established a high performance liquid chromatography method for the determination of 8 lignans in Schisandra.Then,using lignans as the evaluation index,the processing parameters of steamed schisandra,salt schisandra and honey schisandra were investigated,and the best processing technology of each processed product was determined.Thirdly,based on fingerprinting technology combined with similarity analysis,cluster analysis and principal component analysis,the fingerprints of Schisandra chinensis are studied,which can provide reference for the quality evaluation of Schisandra chinensis herbs and processed products.Finally,formulate the processing specifications and quality standards for steamed schisandra,salt schisandra,and honey schisandra,and conduct a preliminary analysis of 5-hydroxymethyl furfural and volatile oil in schisandra and its three processed products.It provides a scientific basis for standardized production,quality control and clinical application of Schisandra and its processed products.更多还原