ABSTRACT
O objetivo pretendido com o presente trabalho foi avaliar a adequabilidade e viabilidade de dois métodos analíticos para quantificação de alprazolam em cápsulas manipuladas: cromatografia líquida de alta eficiência (CLAE) e titulação em meio não aquoso. A quantificação de alprazolam por CLAE fase normal foi realizada em coluna de sílica (30 x 4,6 mm) e fase móvel composta por acetonitrila, clorofórmio, butanol, água e ácido acético glacial (85:8:5:2:0,05). No método titulométrico, as amostras foram dissolvidas em mistura de ácido acético glacial e anidrido acético (3:2) e tituladas com ácido perclórico 0,1 M até o segundo ponto de inflexão. O teor médio de alprazolam obtido por CLAE foi 94,61%, demonstrando a adequabilidade do método proposto. Já as análises por titulação apresentaram teores equivalentes a 128,87% e 91,49% do valor rotulado, devido a interferências detectadas pela presença de excipientes da formulação. A adaptação e o desenvolvimento de métodos analíticos simples e viáveis são de extrema importância para avaliar e garantir a qualidade de medicamentos manipulados, de acordo com as exigências da legislação vigente.
The aim of this study was to assess the suitability and viability of two analytical methods for the quantitation of alprazolam in compounded capsules: high performance liquid chromatography (HPLC) and non-aqueous titration. Quantitation by normal phase HPLC was performed with a silica column (30 x 4.6 mm) and a mobile phase composed of acetonitrile, chloroform, butyl alcohol, water and glacial acetic acid (85:8:5:2:0.05). In the titration method, samples were dissolved in a mixture of glacial acetic acid and acetic anhydride (3:2) and titrated potentiometrically with 0.1 M perchloric acid until the second inflection point. The mean content of alprazolam obtained by HPLC was 94.61% of the label value, showing the suitability of the proposed method. On the other hand, the titration analysis returned contents equivalent to 128.87% and 91.49% of the label value, owing to interference caused by the presence of formulation excipients. The adaptation and development of simple and viable analytical methods are extremely important, in order to assay and ensure the quality of compounded formulations, according to the requirements of the current legislation.
Subject(s)
Alprazolam , Chromatography, Liquid , Pharmaceutical PreparationsABSTRACT
Cimetidine is the selective H2 receptor antagonist and inhibits the secretion of hydrochloric acid in the stomach. In the present study, simple titrimetric method was developed. Respective quantities of Cimetidine were taken in aqueous methanol and acetic acid titrated against 0.1N hydrochloric acid and 0.1N perchloric acid using methyl orange and crystal violet as indicators for neutralization and non-aqueous titrations. All the titrations are carried out by running simultaneous blank determinations. The final titer values are subtracted from blank to get actual amount of acid consumed was determined. These methods were found to be sensitive and inexpensive, do not require any sample processing steps and can be utilized for estimation of cimetidine in bulk and formulations.
ABSTRACT
Objective To set up the reference standard of cyclovirobuxine D.Methods Thermal analysis,HPLC/MS,HPLC with terminal wavelength,HPLC with fluorescence derivation and with ultraviolet derivation,TLC and nonaqueous titration methods were applied to determine the content of cyclovirobuxine D control.Results Thermal analysis can not be used to analyse the purity of cyclovirobuxine D ,and HPLC/MS,HPLC with terminal wavelength,HPLC with fluorescence derivation and HPLC with ultraviolet derivation can obtain the same purity.Conclusion The methods used for the assay of cyclovirobuxine D control were practical.