Part I:1.Analysis of BBI Alkaloids by HPLC 2.Capillary Electrophoretic Separation of BBI Alkaloids Part II:Analysis of Fluoroquinolone Antibacterials by Capillary Electrophoresis

• Main Authors: Wu, An-Cheng, 吳安正
• Other Authors: Sun Shao-Wen
• Format: Others
• Language: zh-TW
• Published: 1997
• Online Access: http://ndltd.ncl.edu.tw/handle/80143281584352045309

碩士 === 國立臺灣大學 === 藥學系 === 85 === This thesis is composed of two parts:Part I : 1. Analysis of Bisbenzylisoquinoline Alkaloids by High Performance Liquid Chromatography2. Capillary Electrophoretic Separation of Bisbenzylisoquinoline AlkaloidsPart II : Analysis of Fluoroquinolone Antibacterials by Capillary ElectrophoresisPart I1. Analysis of Bisbenzylisoquinoline Alkaloids by High Performance Liquid ChromatographyA well-resolved high- performance liquid chromatographic method has been developed for the analysis of nine type VI and type VIII bisbenzylisoquinoline alkaloids ( aromoline, obamegine, berbamine, homoaromoline, colorflammine, thalrugosine, norobaberine, tetrandrine and isotetrandrine. The method used the reversed-phase ion-pair chromatography aided by the photodiode array UV detection. The mobile phase was composed of 27 % volume of acetonitrile and 73 % volume of 0.05 M dihydogen phosphate buffer (pH 3.0) to which 0.1% diethylamine (v/v) and 2 mM sodium heptanesulfonate were added. The method was applied to the analysis of these alkaloids in the stem woods of a Lauraceous plant Dehaasia triandra Merr. Five such alkaloids were identified and their contents were determined. This method should be applicable to the other Lauraceous plants and the various plants containing type VI and type VIII bisbenzylisoquinoline alkaloids.2. Capillary Electrophoretic Separation of Bisbenzylisoquinoline AlkaloidsIn this study, the use of the overlapping resolution mapping scheme to achieve an optimum capillary electrophoretic separation of eight bisbenzylisoquinoline alkaloids, aromoline, obamegine, berbamine, homoaromoline, colorflammine, thalrugosine, tetrandrine and isotetrandrine was investigated. Three critical parameters of electrophoretic media surfactant (sodium cholate), organic modifier (acetonitrile) and pH were chosen to carry out the process. Eight bisbenzylisoquinoline alkaloids were baseline-separated within 20 minutes using the predicted conditions of an optimum separation: buffer containing 132 mM sodium cholate, 25.8% acetonitrile (v/v) and pH 7.58.Part IIAnalysis of Fluoroquinolone Antibacterials by Capillary ElectrophoresisTo meet the requirement of quantitative analysis, this work re-investigated the parameters which were relevant to the separation of the seven fluoroquinolone antibacterials, sparfloxacin, lomefloxacin, norfloxacin, ciprofloxacin, enoxacin, ofloxacin and pefloxacin, based on the method developed previously in this laboratory. With the optimum conditions obtained as follows: electrophoretic media ( 65 mM sodium borate, 35 mM sodium dihydrogen phosphate, 60 mM sodium cholate, pH 7.3 / ACN (72 : 28, v/v); fused silica capillary ( 50 (m I.D., total length 67 cm, effective length 52 cm; injection pressure ( 60 mbar, injection time ( 3 sec; voltage ( 27 kV; detection wavelength ( 275 nm and temperature ( 25℃, the fluoroquinolones were well separated within nine miniutes. After validation with the reproducibility, linearity and accuracy criteria the method was used for the assay of the commercial formulation products. The assay results were within 95~105 % of their labeled claims. The method should be applicable to the analysis of these and other similar formulation products containing these drugs.