蒙药材刺柏叶及其相关制剂的质量控制研究

发布时间：2018-03-10 15:08

本文选题：刺柏叶　切入点：液相指纹图谱　出处：《内蒙古医科大学》2016年硕士论文　论文类型：学位论文

【摘要】：目的:本课题以蒙药材刺柏叶为研究对象,建立液相指纹图谱结合一测多评(QAMS)的质量控制模式和气相指纹图谱分析方法,为全面控制刺柏叶的内在质量提供理论依据;并以刺柏叶中的穗花杉双黄酮、扁柏双黄酮为指标,建立以刺柏叶入药的蒙医经典方药“吉祥安坤丸”的含量测定方法,为刺柏叶在蒙医临床应用提供科学依据。方法:(1)采用高效液相色谱法,以穗花杉双黄酮为参照物,对12批不同来源的刺柏叶进行指纹图谱测定,并建立穗花杉双黄酮与槲皮苷、竹柏双黄酮A、扁柏双黄酮的相对校正因子,通过相对校正因子计算槲皮苷、竹柏双黄酮A、扁柏双黄酮的含量,并与外标法测得值进行比较。(2)采用气相色谱法,以α-蒎烯为参照物,对10批不同来源的刺柏叶进行指纹图谱测定。(3)采用高效液相色谱法,对吉祥安坤丸中刺柏叶所含主要成分穗花杉双黄酮和扁柏双黄酮进行含量测定研究。结果:(1)建立了刺柏叶液相指纹图谱共有模式,标定了16个共有峰,指认了其中5个共有峰:茵芋苷、槲皮苷、穗花杉双黄酮、竹柏双黄酮A、扁柏双黄酮,12批刺柏叶的相似度均在0.95以上;穗花杉双黄酮与槲皮苷、竹柏双黄酮A、扁柏双黄酮的相对校正因子(RCF)依次为2.080、1.383和1.077,相对保留时间(RRT)依次为0.559、1.254和1.303,一测多评法和外标法所得槲皮苷、竹柏双黄酮A、扁柏双黄酮的含量基本一致,相对误差均未超过1.08%。(2)建立了刺柏叶气相指纹图谱共有模式,标定了13个共有峰,10批刺柏叶的相似度均不小于0.90。(3)建立了吉祥安坤丸中穗花杉双黄酮和扁柏双黄酮的含量测定方法,穗花杉双黄酮和扁柏双黄酮的线性范围分别为0.0366~0.366μg,r=0.9999和0.0262~0.262μg,r=0.9999;平均回收率分别为100.9%,RSD=1.22%和99.7%,RSD=1.81%(n=6)。结论:液相指纹图谱与一测多评相结合的质量控制模式用于评价刺柏叶的内在质量即全面准确又具有专属性;以刺柏叶挥发性成分为主的气相指纹图谱可与液相指纹图谱的信息互为补充,更好的评价药材的品质;吉祥安坤丸中的穗花杉双黄酮和扁柏双黄酮均为刺柏叶的主要活性成分,所建立的含量测定方法简单易行,可为刺柏叶用于吉祥安坤丸的定量研究提供参考。
[Abstract]:Objective: to establish a quality control model and a gas phase fingerprint analysis method based on liquid phase fingerprint and QAMS to provide a theoretical basis for the overall control of the internal quality of Cypress chinensis leaves. The content determination method of "Jixiang Ankun pills", a classical Mongolian medicine, was established on the basis of the index of Chinese fir bisflavone and cypress diflavonoids in the leaves of Cypress chinensis, and the content of them was determined by the traditional Mongolian medicine "Jixiang Ankun Pill". To provide scientific basis for the clinical application of cypress leaf in Mongolian medicine. Methods the fingerprint of 12 batches of Chinese cypress leaves from different sources was determined by high performance liquid chromatography (HPLC) and quercetin from different sources were established. The contents of quercetin, cypress bisoflavone A and cypress diflavonoids were calculated by relative correction factor, and compared with those obtained by external standard method. Using 伪 -pinene as the reference material, 10 batches of Chinese cypress leaves from different sources were determined by HPLC. The contents of bisflavone and bisflavone in the leaves of Cypress chinensis were determined in Jixiang Ankun Pill. Results the common pattern of liquid phase fingerprint of Cypress chinensis leaves was established, and 16 common peaks were calibrated. Among them, five common peaks were identified: the similarity of the leaves of 12 batches of Artemisia chinensis, quercetin, fir bisflavone, cypress bisoflavone A and cypress diflavone were all above 0.95, and the similarity between them was more than 0.95, and the similarity between them was more than 0.95, and the similarity between them was above 0.95. The relative correction factors (RCFs) were 2.080 and 1.077, and the relative retention time (RRTT) were 0.559n1.254 and 1.303, respectively. The contents of quercetin, diflavonoids A and diflavonoids were basically the same as those obtained by multi-evaluation method and external standard method. The common pattern of gas phase fingerprint of cypress leaf was established, and the similarity of 10 batches of Cypress chinensis in 13 common peaks was calibrated. The similarity was not less than 0.90.93) the method for the determination of bisflavone and diflavone in Jixiang Ankun Pill was established. The linear ranges of bisflavone and cypress bisflavone were 0.0366n 0.366 渭 g ~ 0.9999 and 0.0262 ~ 0.262 渭 g ~ 0.262 渭 g ~ (0.9999), respectively. The average recoveries were 100.9% RSD1. 22% and 99. 7% RSD1. 81% respectively. Conclusion: the quality control model combined with liquid fingerprint and multiple evaluation was used to evaluate the internal quality of leaves of Cypress przewalskii. It is comprehensive, accurate and exclusive. The gas phase fingerprint with the volatile components in the leaves of Cypress chinensis can complement the information of the liquid fingerprint, and better evaluate the quality of the medicinal materials, and the bisflavone of Chinese fir in Jixiang Ankun pills is the main active components of the leaves of Cypress przewalskii. The established method is simple and practical and can be used for quantitative study of Jixiang Ankun pills.
【学位授予单位】：内蒙古医科大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：R29

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