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.
Asunto(s)
Albendazol/análogos & derivados , Albendazol/química , Albendazol/aislamiento & purificación , Amilosa/análogos & derivados , Amilosa/química , Cromatografía Líquida de Alta Presión/métodos , Fenilcarbamatos/química , Isomerismo , Transición de FaseRESUMEN
The relationships of gastric cancer with serum trace elements, helicobacter pylori (HP) and COX-2 in gastric tissue were investigated. We took 50 blood samples from the gastric cancer patients in Hexi region (the gastric cancer group), and 50 blood samples from healthy volunteers (control group) and detected the level of trace elements, the rate of HP infection, and the expression of COX-2 in gastric tissue. The results showed the levels of Cu/Zn, Fe in the serum of the gastric cancer group were higher than those of the control group respectively(P < 0.05, 0.01), and the levels of Zn, Mn were lower than those of the control group respectively (P < 0.05, 0.01). The data on Zn were submitted to multi-variate non-conditional logistic analysis. The rate of HP infection and the positive expression of COX-2 were 88% and 78% respectively in the gastric cancer group, 42.0% and 0 in the control group (P < 0.01). These findings suggest that the decrease of Zn in serum may be a precancerous factor of gastric cancer development which induces HP infection and the higher expression of COX-2 and hence may lead to the development of gastric cancer. Detecting the trace elements could conduce to the diagnosis of gastric cancer. Regulating the level of trace element in the patient can be an effective chemoprophylaxis for gastric cancer.
Asunto(s)
Adulto , Femenino , Humanos , Masculino , Persona de Mediana Edad , Estudios de Casos y Controles , Ciclooxigenasa 2 , Metabolismo , Infecciones por Helicobacter , Metabolismo , Helicobacter pylori , Modelos Logísticos , Factores de Riesgo , Neoplasias Gástricas , Sangre , Metabolismo , Microbiología , Oligoelementos , Sangre , Zinc , SangreRESUMEN
A high performance liquid chromatographic (HPLC) method using triethylamine (TEA), copper *" acetate and L-proline as the chiral mobile phase (CMP) and the enantiomric analysis of thyroxine (T4) are described. The influence of the mobile phase parameters including the TEA concentration, manipulation pH, concentration of Cu*", concentration of L-proline, temperature of column and flow rate of eluent on the enantiomers separation of thyroxine was studied. The HPLC-CMP is a simple method for separation and determination of D，L-T4 in drug or in human plasma. It can be used to therapeutic drug or adverse drug reactions monitor.
