RESUMEN
The presented developed HPLC method and GC method may be used to separate and determine all analyzed 3-hydroxy-3-methylglutaryl-coenzyme A reductase inhibitors (statins) and ezetimibe using a single columns and a uniform methodology. In order to perform qualitative and quantitative tests of statins and ezetimibe the Symmetry C18 column 250 mm x 4.6 mm, 5 µm, the mobile phase: acetonitrile:water (70:30, v/v), adjusted to pH = 2.5 and a spectrophotometric detector for the HPLC method were used. For GC method column HP-1; 30 m x 0.25 mm x 0.25 µm and FID detector were selected. All results and statistical data obtained indicate good method sensitivity and precision. The RSD values are appropriate for both newly developed methods.
Asunto(s)
Anticolesterolemiantes/análisis , Cromatografía de Gases/métodos , Cromatografía Líquida de Alta Presión/métodos , Ezetimiba/análisis , Inhibidores de Hidroximetilglutaril-CoA Reductasas/análisisRESUMEN
Benazepril hydrochloride contains two stereogenic centers, but is currently available as single enantiomer (S,S configuration) for the treatment of hypertension. Its enantiomer (R,R configuration) and the diastereoisomeric pair (R,S and S,R) can be regarded as impurities. Stereochemical stability of S,S isomer of benazepril hydrochloride and its potential susceptibility to conversion in the.active substance and in Lisonid tablets were examinated. The separation with the use of the TLC method with the following system: chromatographic plates Chiralplate and a mobile phase: methanol - acetonitrile - 1 mM copper(II) acetate (4 : 2 : 4, v/v/v) with saturation of glacial acetic acid for 1 h and the HPLC method system: Chiral AGP column (150 x 4.0 man x 5 µm) and a mobile phase: phosphate buffer pH = 6.0 - methanol (80 : 20, v/v) were obtained. Active substance - benazepril hydrochloride and Lisonid tablets 20 mg were subjected to the impact of different stress factors. Samples were examined after 1 and 6 weeks. It was found that none of the applied stress factors caused the transformation of the S,S enantiomer of benazepril hydrochloride in the substance and tablets to other identified stereoisomers - only the compound decomposition has occurred.
Asunto(s)
Antihipertensivos/química , Benzazepinas/química , Cromatografía Líquida de Alta Presión , Cromatografía en Capa Delgada , EstereoisomerismoAsunto(s)
Anticolesterolemiantes/análisis , Colesterol/sangre , Cromatografía Líquida de Alta Presión , Ácidos Fíbricos/análisis , Inhibidores de Hidroximetilglutaril-CoA Reductasas/análisis , Hiperlipidemias/tratamiento farmacológico , Anticolesterolemiantes/uso terapéutico , Biomarcadores/sangre , Calibración , Cromatografía de Gases , Cromatografía Líquida de Alta Presión/normas , Ácidos Fíbricos/uso terapéutico , Inhibidores de Hidroximetilglutaril-CoA Reductasas/uso terapéutico , Hiperlipidemias/sangre , Estándares de ReferenciaRESUMEN
With reference to common application of HPLC to routine analytical tests on medicinal products decreasing the level of cholesterol, including three compounds from this group--fenofibrate, bezafibrate and etofibrate, we developed a new method for determining two other compounds--ciprofibrate and gemfibrozil. The developed HPLC method may be used for identification and qualitative determination of selected compounds--derivatives of aryloxyalkylcarboxylic acids as well as it may be used for simultaneous separation and determination of all compounds from the group of fibrates using one column and the same methodology. The results and statistical data indicate good sensitivity and precision. The RSD value presented is equivalent to the newly developed method of determinination of ciprofibrate and gemfibrozil in the substances and medicinal products--capsules and coated tablets.
