Development and validation of HPLC method for analysis of dexamethasone acetate in microemulsions

Abstract

A simple, rapid, accurate and sensitive method was developed for quantitative analysis of dexamethasone acetate in microemulsions using high performance liquid chromatography (HPLC) with UV detection. The chromatography parameters were stainless steel Lichrospher 100 RP-18 column (250 mm x 4 mm i.d., 5 µm particle size), at 30 ± 2 ºC. The isocratic mobile phase was methanol:water (65:35; v/v) at a flow rate of at 1.0 mL.min -1. The determinations were performed using UV-Vis detector set at 239 nm. Samples were prepared with methanol and the volume injected was 20 µL. The analytical curve was linear (r 2 0.9995) over a wide concentration range (2.0-30.0 µg.mL -1 ). The presence of components of the microemulsion did not interfere in the results of the analysis. The method showed adequate precision, with a relative standard deviation (RSD) smaller than 3%. The accuracy was analyzed by adding a standard drug and good recovery values were obtained for all drug concentrations used. The HPLC method developed in this study showed specificity and selectivity with linearity in the working range and good precision and accuracy, making it very suitable for quantification of dexamethasone in microemulsions. The analytical procedure is reliable and offers advantages in terms of speed and low cost of reagents. Um método simples, rápido, preciso e sensível foi desenvolvido para a análise quantitativa de acetato de dexametasona em microemulsões usando cromatografia líquida de alta eficiência (CLAE). Os parâmetros cromatográficos foram: coluna cromatográfica Lichrospher 100 RP-18, (250 mm x 4 mm i.d., 5 µm partícula tamanho), com temperatura de coluna de 30 ± 2 ºC. A fase móvel foi composta de metanol: água (65:35; v/v) com fluxo isocrático de 1 mL.min -1 e volume de injeção de 20 µL. As determinações foram realizadas utilizando detector UV-Vis no comprimento de onda de 239 nm. A curva analítica mostrou-se linear (r 2 0,999) em uma ampla faixa de concentração (2,0-30,0 µg.mL -1 ). A presença de componentes da microemulsão não interferiu nos resultados da análise. O método mostrou precisão adequada, com desvio padrão relativo menor que 3%. A exatidão foi analisada pela adição de padrões do fármaco e valores de recuperação dentro dos limites recomendáveis foram obtidos para todas as concentrações estudadas. O método por CLAE mostrou especificidade e seletividade com linearidade dentro da faixa de concentração utilizada e precisão e exatidão que tornam o método adequado para a análise de dexametasona em microemulsões. O procedimento analítico é fidedigno e oferece vantagens em termos de velocidade e custo de reativos. Unitermos: Acetato de dexametasona/determinação. Microemulsões/análise quantitativa. Cromatografia líquida de alta eficiência/análise quantitativa. Método de análise/validação.

Stability Indicating Rp-HPLC Method for Simultaneous Determination of Ciprofloxacin and Dexamethasone in Binary Combination

“…Dexamethasone (8S,9R,10S,11S,13S,14S,1 6R,17R)-9-Fluoro-11,17-dihydroxy-17-(2-hydroxyacetyl)-10,13,16-trimethyl-, 7,8,9,10,11,12,13,14,15,16,17-dodecahydro-3H-cyclopenta[a] phenanthren-3-one [ Figure 1] a corticosteroid, is used to relieve bacterial ocular infections that require corticosteroid [1]. Many authors have reported a lot of different analytical methods for both drugs individually utilizing different techniques like HPLC [2][3][4][5][6][7][8][9], spectrophotometry and spectrofluorometric [10][11][12][13], titrimetric [14] methods for ciprofloxacin while for dexamethasone different methods involving HPLC, GC and TLC are reported [15][16][17][18][19][20][21].…”

Development and Validation of an Hplc Method for Voriconazole Active Substance in Bulk and its Pharmaceutical Formulation

“…to evaluate the specificity of the analytical method, the blank and drug loaded pharmaceutical formulation has been injected into the chromatographic system. These parameters were determined by comparing the chromatograms of the voriconazole standard, drug loaded in situ gel and blank in situ gel (15).…”

Quantification of Andrographolide Isolated from <i>Andrographis paniculata</i> Nees Obtained from Traditional Market in Yogyakarta Using Validated HPLC

“…Consequently, linearity, precision, specificity, accuracy, sensitivity, and quantification limit must be demonstrated in the test for analysis adequacy [16,17]. The objective of present work is to quantification of andrographolide isolated from A. paniculata Ness found in a traditional market in Yogyakarta using validated HPLC to obtain high-level content of andrographolide.…”