RESUMEN
A microemulsion electrokinetic chromatographic (MEEKC) method has been developed and validated for determination of resibufogenin and cinobufagin in toad venom and in traditional Chinese medicine prepared from the venom. The MEEKC method involved use of sodium dodecyl sulfate (SDS) as surfactant, heptane as organic solvent, and butan-1-ol as co-solvent. To improve the separation, the effect of temperature and running buffer pH were evaluated. The optimized conditions (heptane 0.81% (w/w), SDS 3.31% (w/w), butan-1-ol 6.61% (w/w), and 10 mmol L(-1) sodium tetraborate buffer, pH 9.2, and 298 nm as the detection wavelength) enabled useful and repeatable separation of the analytes.
Asunto(s)
Venenos de Anfibios/química , Bufanólidos/análisis , Electrocromatografía Capilar/métodos , Medicina Tradicional China , Preparaciones Farmacéuticas/química , Animales , Anuros , Electrocromatografía Capilar/instrumentación , Emulsiones/química , Concentración de Iones de Hidrógeno , Conformación Molecular , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Dodecil Sulfato de Sodio/química , Estereoisomerismo , Temperatura , Factores de TiempoRESUMEN
The present paper describes the development of a microemulsion electrokinetic chromatographic (MEEKC) method for simultaneous determination of andrographolide and dehydroandrographolide in traditional Chinese medicines and Chinese medicinal preparations. The MEEKC method involved the use of sodium dodecyl sulfate (SDS) as surfactant, heptane as organic solvent and butan-1-ol as co-solvent. The effect of temperature and pH of running buffers on separation were examined. The optimized conditions (heptane 0.81% (w/w), SDS 3.31% (w/w), butan-1-ol 6.61% (w/w) and 10mM sodium tetraborate buffer, pH 9.2) allowed a useful and good reproducible separation of the studied analytes to be achieved.
Asunto(s)
Andrographis/metabolismo , Química Farmacéutica/métodos , Cromatografía Capilar Electrocinética Micelar/métodos , Diterpenos/análisis , Medicamentos Herbarios Chinos/análisis , Antiinflamatorios no Esteroideos/análisis , Butanoles/química , Calibración , Técnicas de Química Analítica/métodos , Emulsiones , Concentración de Iones de Hidrógeno , Modelos Químicos , Preparaciones Farmacéuticas/análisis , Dodecil Sulfato de Sodio/química , Solventes , Temperatura , Factores de TiempoRESUMEN
Broad spectrum anthelmintic agent-albendazole sulfoxide (ABZSO) have been separated and semiprepared on amylose tris (3,5-dimethylphenylcarbamate) chiral stationary phases by HPLC using mobile phases contained with n-hexane and different alcohols. For analytical separation the influence of the nature and content of alcoholic modifiers on separation were systemically studied. Then, the analytical methods were scaled up to semipreparative loading to obtain small quantities (about 1 g) of both ABZSO enantiomers. Especially, different loading amounts were investigated for their effect on various parameters of semipreparative HPLC. In addition, optical rotation and circular dichroism (CD) of both ABZSO enantiomers collected were determined and single enantiomers were found stable in configuration for 1 year.