| There are five parts in this article. The development and applications of High Performance Capillary Electrophoresis (HPCE) and High Performance Liquid Chromatography (HPLC) in pharmaceutical analysis are reviewed in recent years. Diacerein, anthraquinone and Tamsulosin Hydrochloride are analysed by HPCE and HPLC.In the first chapter, the development and applications of HPCE and HPLC in pharmaceutical analysis are reviewed.In the second chapter, establishing an HPCE-LIF method for separation and determination of the intermediate of tamsulosin hydrochloride, (R/S)-5-(2-aminopropyl)-2-methoxybenzenesulfonamide (R/S-APMB). (R)-5-(2-aminopropyl)-2- methoxy-benzenesulfonamide can react with fluorescein isothiocyanate (FITC) and then FITC-R-APMB was achieved. FITC-R-APMB was separated using 70mmol·L-1 borate as buffer. The uncoated fused-silica capillary of 15μm i.d and 47cm length (effective length 40cm) was used. The capillary temperature was maintained at 20℃.Samples were injected with pressure at 3.45kPa for 1s and separated at 20kV. Both R- and S-APMB had low detection limits (8.2×10-9mol·L-1). The linear range of R- APMB was 8.20×10-8-9.02×10-7 mol·L-1.The method is simple and offers a high sensitivity. And it can be used to control the production of tamsulosin.In the third chapter, establishing an analytical method of HPCE to separate Diacerein and Rhein and determine the content of Diacerein in Artrodar. Untreated fused-silica capillary (75μm×57cm, effective length is 50cm) was used. Pressure injection of 0.5psi×3sec was employed, and the temperature was 30℃. The detection wavelength was set at 261 nm. The sample was analyzed with running buffer of 10mmol·L-1 borate and 10mmol·L-1 sodium biphosphate (pH=7.0) at 20kV voltage. The calibration curve of Diacerein showed good linearity over the range of 0.0229-0.538mmol·L-1 (r=0.996). The average recoveries of the method were 98.9% (n=5). The method is simple, rapid and reproducible and can be applied in the determination of Diacerein in Artrodar.In the forth chapter, a method was established for the determination of anthraquinone by HPLC. The analysis was carried out with Kromasil C18 (4.6×150 mm, 5μm) Column,using MeOH-H2O-H3PO4 (92 : 8 : 0.5) as the mobile phase. The flow rate was 1.0mL/min, the detection wavelength was set at 254nm and the column temperature was maintained at room temperature. The method was proved to be specific, accurate and convenient. The proposed RP-HPLC method could be used for the determination of anthraquinone.In the fifth chapter, establishing an RP-HPLC method for determination of Diacerein in Artrodar. Kromasil C18 ( 4.6×150mm, 5μm ) was used, and the mobile phase consisted of MeOH-H2O-H3PO4 ( 69.5 : 30 : 0.5). The flow rate was 0.8mL/min and the determination wavelength was at 261nm. The linear range was in the range of 0.0101-0.101mg/ml (r= 0.999). The average recoveries were 101%; RSD were 1.35% (n = 4). This method is simple, rapid and reliable for determination of Diacerein.
|
PDF Full Text Request