ABSTRACT
Objective: To establish the method for determination of taurocholic acid in the Traditional Chinese Medicine Shedanchuanbei Oral Liquid and snake bile. Methods: The sample was prepared as mixed solution containing methanol and KH 2PO 4. The mixed solution was injected into Sep Pak C 18 cartridge for the purpose of sample purity. In this processing, the substances which having strong retain action and could harm analytic column were hold in the Sep Pak C 18 cartridge. The eluting solution that the Sep Pak C 18 cartridge had be over loading for taurocholic acid was used as the test solution. The test solution was measured by RP HPLC. The chromatographic conditions were as followed: Supelcosil LC 8 column(150mm?4.6nm,5?m) as analytic column, detect wavelength at 203nm, and MeOH 0.4%KH 2PO 4 mixed solution(56∶44, V/V ) as mobile phase. The inject volume was 50?L. Results: The linear response range of sodium taurocholate was from 0.0253mg?mL -1 to 0.253mg?mL -1 , and the correlation coefficient was 0.9999. The average recovery rate was 101.3%, RSD was 0.40%( n =6). Conclusion: This method was simple, efficient and suitable to the quality control for Shedanchuanbei Oral Liquid and snake bile.
ABSTRACT
Objective: To establish a method for the determination of metamizole sodium and chlorphenamine malete in zhongganling Tablets. Methods: The sample was determined by ion pair HPLC after it was purified on Sep Pak C 18 microcolumn. The chromatographic conditions included: Hypersil DBS C 18 chromatographic column (250mm?4.6mm, i.d.5?m) as an anlaytical column, methanol mixed solution of sodium heptanesulfonate and glacial acetic acid (600∶400) as a mobile phase, the detection wavelength at 264nm and 1.0mL?min -1 of flow rate. Results: The average recoveries of metamizole sodium and chlorphenamine maleate were 99.6% (RSD was 2.1% and n was 6) and 98.0% (RSD was 1.5% and n was 6), respectively. Conclusion: Metamizole sodium and chlorphenamine maleate can be determined respectively by HPLC with the same mobile phase when Sep Pak C 18 microcolumn solid phase extraction method is used to substitute for the traditional sample pretreatment methods refluxing, extracting and concentrating, and sodium heptanesulfonate ion pair reagent in acid condition is selected.