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HPLC在药物分析及中药指纹图谱研究中的应用

Application of HPLC in Pharmaceutical Analysis and Chinese Medicine Fingerprint

【作者】 钟东会

【导师】 雷根虎;

【作者基本信息】 西北大学 , 分析化学, 2004, 硕士

【摘要】 本文研究了高效液相色谱(HPLC)在苦参、白芍和薏辛除湿止痛胶囊及龙胆苦甙在犬体内代谢时含量的测定分析方法,并对酸枣仁皂甙的提取富集及其药材指纹图谱的建立进行了研究,由以下六部分组成: (一) 综述 对近年来高效液相色谱法在药物分析及中药指纹图谱研究中的应用进行了文献综述。 (二) 苦参药材中苦参碱类物质的提取与HPLC测定方法的研究 本文研究了不同产地苦参中生物碱含量的HPLC测定方法,并对其提取溶剂、提取时间、柱温进行了优化。结果表明:以氯仿(氨性)为提取溶剂超声提取三十分钟、柱温控制在20~25℃为最适宜条件,方法回收率在94.68%~103.10%之间,相对标准偏差为0.58%~1.47%,该方法快速、灵敏、准确,可为不同产地的苦参质量控制提供依据。 (三) RP-HPLC测定芍药及薏辛除湿止痛胶囊中芍药苷的方法研究 本文采用L9(34)正交试验对提取方式进行优化,建立芍药及薏辛除湿止痛胶囊中芍药苷的HPLC测定方法。结果表明:40倍量的水饱和的正丁醇超声提取三次,每次30min为最佳提取方式。方法回收率分别为102.82%和101.03%,相对标准偏差分别为3.68%和1.8%,该方法准确、灵敏、高效,有实用价值,可作为该制剂质量控制的方法。 (四) RP-HPLC法测定犬的肝、肾和血清中龙胆苦甙的方法研究 本文采用醇沉离心的方法对组织进行前处理,研究了龙胆苦甙在犬体内代谢时含量的HPLC测定方法。结果表明:该方法精密度和回收率比较高,线性和重现性都比较好,符合一般药代动力学研究的要求,建立了简便、灵敏的HPLC-UV检测法以定量分析生物组织、体液中的龙胆苦甙,是一种较理想的测定犬体内龙胆苦甙含量的方法。 (五) 酸枣仁中有效成分的提取与富集方法的研究百北大学硕士毕习匕引仑文 本文采用与(34)正交试验对提取方式进行优化,同时采用大孔吸附树脂对酸枣仁皂贰进行富集纯化。结果表明:水浴回流的提取率高于超声的提取率,大孔树脂的富集率达到了89.26%,回收率在90.28一100.02%之间,相对标准偏差为4.18%,该方法准确、灵敏、有实用价值,可作为富集纯化酸枣仁皂贰及含量测定的方法用。 (六)酸枣仁药材指纹图谱分析方法研究及不同产地药材谱比较 本文通过对流动相梯度洗脱系统的考察及10批不同产地脱脂酸枣仁药材样品的甲醇提取液的色谱图的分析,建立了酸枣仁药材的HPLC指纹图谱。应用相对保留值来分析样品之间的差异。结果表明:该方法精密度高、重现性好,可作为评价和控制其不同产地酸枣仁药材质量的标准。

【Abstract】 This thesis studies on the methods of determination for Sophora flovescens Ait, Yixin Chunshi Zhitong Capsules and gentiopicroside in animal tissue by HPLC, what’s more, the extracting enrichment of Jujubaside and its HPLC fingerprint has been studied. It includes six parts as follows: Part I Review.A review of HPLC is applied to pharmaceutical analytic and Chinese medicine fingerprint.Part II Study of the extracting alkaloids in Sophora flovescens Ait and determining method by HPLCThe method of the quantity of three alkaloids in differene Sophora flovescens Ait has been determined by HPLC. At the same time, by optimizing with the condition to the extracting solvent, extracting time, the column temperature. It was resulted that the condition was good by CH3Cl(being extracting solvent)extracting thirty minutes and control the column temperature between 20 and 25C. The recoveries ranged from 94.68%~103.10%.RSD was 0.58%~1.47%, The method is rapid, sensitive and suitable to control the quality of the Sophora flovescens Ait in different area.Part III: Determination of paeoniflorin in Paeoria lactiflora Pall, and Yixin Chunshi Zhitong Capsules by HPLC.The extracting method has been optimized by orthogonal experimental factor and levels. The HPLC method determines paeoniflorin in Paeoria lactiflora Pall, and Yixin Chunshi Zhitong Capsules. The results show that the butanol with the saturating water extracts three times by ultrasonic, each time using half an hour. The respective recoveries was 102.82% 101.03%, RSD was 3.68% 1.8%, The method is rapid, sensitive and suitable to control the quality of the peony and its preparation.Part IV: Determination of gentiopicroside in Dog liner, kidney, and blood serum by HPLC.The method of centrifugal sedimentation has been used in predisposaling tissue. The metabolizing of gentiopicroside’s concentration in the body of dog has been determined by the HPLC. The present method has high recovery and precision, with a good liner and reproductividy, which is suit for the analysis of the metabolizing of pharmaceutical in animal’tissue. The method is rapid, sensitive and suitable to determine the quantity of the gentiopicroside within the dog.Part V : Study of the extraction and enrich the effective component in the seed of Ziziphus jujubaMill var.Spinosa.The extracting method has been optimized by orthogonal experimental factor and levels, at the same time,by using the Macroporous Adsorptive resins to enrich and pure Jujubaside. The results show that the extracting rate of waterheat is higher than the ultrasonic’s. The Macroporous Adsorptive resins has high enrichment, obtaining to 89.26%. The recoveries ranged from 90.28%~100.02%, RSD was 4.18%, The method is rapid, sensitive and suitable to enrich and control the quality of the Jujubaside in the seed of Ziziphus jujubaMill var.Spinosa(Bunge) Hu ex H. F. chou.Part VI: Study on HPLC-FPS Analysis of the seed of jujubaMill var.Spinosa and comparative study on its different sourcesThis article establishs the HPLC fingerprinter of the seed of Ziziphus jujubaMill var.Spinosa(Bunge) Hu ex H. F. chou. By experimentizing the grads system of the fluid and analyzing the chromatogram on ten batch samples. The parameter of relative retention value(time, area)is used to study the difference between the ten batch of samples. The results show that the method is good precision and reproductividy, which is suitable to assess and weigh the quality of the Ziziphus jujubaMill var.Spinosa(Bunge) Hu ex H. F. chou.Zhong DongHui (analytical chemistry) Directed by Lei Genhu

  • 【网络出版投稿人】 西北大学
  • 【网络出版年期】2004年 04期
  • 【分类号】O657.7;TQ460
  • 【被引频次】1
  • 【下载频次】874
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