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紫锥菊、杜仲等的LC/MS方法研究及相关标准对照品的制备

Methodology Studies of Echinacea and Eucommia Ulmoides et al by LC/MS and Preparations of Related Standards

【作者】 罗旭彪

【导师】 姚守拙; 陈波;

【作者基本信息】 湖南师范大学 , 有机化学, 2003, 硕士

【摘要】 大气压电离质谱的出现,成功地解决了液相色谱和质谱联用的接口问题,使液相色谱.质谱联用(LC-MS)逐渐发展成为成熟的技术。液相色谱/质谱集LC的高分离能力与MS的高灵敏度、极强的专属性于一体,广泛地应用于植物化学、分析化学、药学、生物化学、临床医学、农药残留等领域。 本论文主要研究内容如下: 1.以高效液相色谱、二极阵列管紫外检测器和电喷雾质谱检测器联用方法来同时分析紫锥菊Echinacea Purpurea(L)Moench.中咖啡酸衍生物和异丁酰胺类化合物。从而建立了一种更全面的紫锥菊药材及其提取物的质量控制方法。 2.首次应用醋酸铵-甲醇组成流动相与C18反相柱、二极阵列管检测器分析菊苣酸。流动相简单,方法精密度高,分离效果好,准确、快速。对紫锥菊及其复方制剂中菊苣酸的含量进行了分析,结果满意。 3.基于液质联用能在线提供结构信息、灵敏度高的特点,发展了一种对杜仲Eucommia ulmoides中九种活性组分定性、定量的方法。将这个方法应用于杜仲的皮、叶、提取物、天麻杜仲胶囊和杜仲茶中九种活性成分的检测,获得了满意的结果。 4.采用高效液相色谱/大气压化学电离质谱法,对博落回果Macleaya cordata(Willd.)R.Br.中生物碱进行定性和定量分析,得到满意的结果;并且得到了博落回果实的液相色谱/质谱的指纹特征图谱。 5.采用低压反相制备色谱对紫锥菊提取物中菊苣酸、人参根提取物中人参二醇类皂贰、人参三醇类皂贰的分离制备进行了初步探讨。

【Abstract】 With the emergence of atmospheric pressure ionization (API), combined high performance liquid chromatography and mass spectrometry (LC/MS) technique has been rapidly developed in past two decades. It takes advantages of chromatography as a high performance separation method and of both photodiode array detection (DAD) and MS as a sensitive identification method. Its applications have been extended to phytochemistry, analytical chemistry, biochemistry, clinical and pharmacological researches and so on.The studies in this thesis are summarized as follows:1. An HPLC-DAD-ESIMS method was developed for the simultaneous analysis of caffeic acid derivatives and alkamides in the roots and extracts of Echinacea purpurea. The method is better than previously published techniques in product quality control, and can provide HPLC fingerprints of bio-active components in Echinacea purpurea.2. An HPLC-DAD method for the determination of cichoric acid in Echinacea purpurea was reported by use of 400 mmol/L ammonium acetate-methanol (95:5) as mobile phase. The method was simple, sensitive, accurate and precise, and had been successfully applied in the determination of cichoric acid in Echinacea purpurea. L. extract and Echinacea purpurea. L. preparations.3. A rapid, specific and reproducible HPLC-DAD- ESIMS technique was developed for the determination of nine bioactive compounds in Eucommia ulmoides Oliv. The newly developed technique has been used for the rapidanalysis of a number of samples includingEucommia ulmoides cortex, leaves, extracts, mixed preparations of traditional Chinese patent medicines and beverages. This method can be used for quality control of medicinal materials of Eucommia ulmoides Oliv and its preparations.4. An HPLC/APCIMS method for separation and determination of alkaloids in Macleaya cordata (Willd.) R. Br. was established. HPLC/APCIMS fingerprints of alkaloids in Macleaya cordata (Willd.) R. Br. were obtained.5. Purification and separation of cichoric acid, panaxtriols and panaxadiols by preparative HPLC were discussed.

  • 【分类号】O657.63
  • 【被引频次】1
  • 【下载频次】529
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