Quantitative analysis of ursodeoxycholic acid in pharmaceutical preparation by capillary electrophoresis with indirect UV detection

• Main Author: 張幸運
• Other Authors: 孫紹文
• Format: Others
• Language: zh-TW
• Published: 2000
• Online Access: http://ndltd.ncl.edu.tw/handle/73550465306562280547

碩士 === 國立臺灣大學 === 藥學研究所 === 88 === 英文摘要 This thesis is composed of two parts: Part I: Quantitative analysis of ursodeoxycholic acid in pharmaceutical preparation by capillary electrophoresis with indirect UV detection Part II:Separation of lignans by micellar electrokinetic capillary chromatography Part I Quantitative analysis of ursodeoxycholic acid in pharmaceutical preparation by capillary electrophoresis with indirect UV detection The aim of this study was to develop a simple and rapid capillary electrophoretic method, with indirect UV detection, for the quantification of ursodeoxycholic acid (UDCA) in pharmaceutical preparations. Sodium p-hydroxy benzoate was used as buffer electrolyte (pH 8.0) and background-providing chromophore (visualization agent). Separation was carried out on a fused-silica capillary (50 mm ´ 72 cm) at a potential of 25 kV under ambient temperature (23 ± 2°C) and detected at 250 nm. Glycocholic acid was used as internal standard for quantification. Both run-to-run repeatability and day-to-day reproducibility of migration time were below 0.1% RSD. The repeatability and reproducibility of relative peak height were 3.8% and 4.8% RSD, respectively. The accuracy tested by recovery of two pharmaceutical preparations was 99.52% and 102.47%, respectively. The linearity of relative peak height was tested in the range 20~100 mg ml-1. The limit of detection was found to be 3 mg ml-1. The method can be used to assay UDCA raw materials and formulation products. Part II Separation of lignans by micellar electrokinetic capillary chromatography This study was aimed to establish a rapid capillary electrophoretic method to facilitate the study of lignans rich in some Euphorbiaceous plants, especially the Phyllanthus genus. Twelve lignans isolated from P. urinaria and P. myrtifolius were taken as analytes to perform their separation by micellar electrokinetic capillary chromatography. It was found that the surfactant was critical to optimal separation and sodium deoxycholate was most appropriate to such purpose. Five parameters including pH value, buffer concentration, surfactant concentration, organic modifier and applied voltage were investigated to evaluate their effects on separation. Optimum separation conditions were found as follows: fused silica capillary- 50 mm ´ 72 cm, effective length 60 cm; voltage- 24 kV; electrophoretic media- 15 mM sodium dihydrogen phosphate, 10 mM sodium borate, 15 mM sodium deoxycholate, pH 8.7; detection wavelength- 230 nm and operation temperature- 35°C. Baseline separation of these twelve lignans was achieved within 12 minutes.