Spectrophotometric and HPLC determination of deflazacort in pharmaceutical dosage forms

Abstract

(DFZ) is a glucocorticoid used as an anti-inflammatory and immunosuppressant drug. No official methods are available for DFZ determination in pharmaceutical formulations. The objective of this study was to develop, validate and compare spectrophotometric (UV and colorimetric) and highperformance liquid chromatography (HPLC) methods, for the quantitative determination of DFZ in tablets and oral suspension. For the UV method, ethanol was used as the solvent, with detection at 244 nm. The colorimetric method was based on the redox reaction with blue tetrazolium in alkaline medium, with detection at 524 nm. The method by HPLC was carried out using a C 18 column, mobile phase consisting of acetonitrile:water (80:20, v/v) with a flow rate of 1.0 mL min -1 and detection at 244 nm. The methods proved linear (r > 0.999), precise (RSD < 5%) and accurate (recovery > 97%). Statistical analysis of the results indicated that the UV and HPLC methods were statistically equivalent, while the values obtained for the colorimetric method differed significantly from the other methods. O deflazacorte (DFZ) é um fármaco glicocorticóide usado como antiinflamatório e imunossupressor. Métodos oficiais não estão disponíveis para a determinação de DFZ em formas farmacêuticas. Este estudo teve como objetivo desenvolver, validar e comparar métodos por espectrofotometria (UV e colorimetria) e cromatografia líquida de alta eficiência (CLAE), na determinação quantitativa de DFZ em comprimidos e suspensão oral. O método por UV utilizou etanol como solvente, com detecção em 244 nm. O método colorimétrico foi baseado na reação de redução com azul de tetrazólio em meio alcalino, com detecção em 524 nm. O método por CLAE utilizou coluna C 18 ; fase móvel constituída de acetonitrila:água (80:20, v/v), com fluxo de 1,0 mL min -1 e detecção em 244 nm. Os métodos foram lineares (r > 0,999); precisos (RSD < 5 %), e exatos (recuperação > 97%). As análises estatísticas dos resultados obtidos indicaram que os métodos por UV e por CLAE foram estatisticamente equivalentes, enquanto os valores obtidos para o método colorimétrico diferiram significativamente dos demais métodos.Unitermos: Deflazacorte/determinação quantitativa. Cromatografia líquida de alta eficiência/análise quantitativa. Espectrofotometria/análise quantitativa. Medicamentos/análise quantitativa.

Nanoencapsulation of a glucocorticoid improves barrier function and anti-inflammatory effect on monolayers of pulmonary epithelial cell lines

“…Loading rate was determined after dissolution of an aliquot (200 µl) of nanocapsules suspension in 10 ml of mobile phase followed by ultrasound for 10 min and quantified by liquid chromatography (LC) using a previously validated methodology [21]. The chromatographic system consisted of a Gemini RP-18 column (250 mm x 4.6 mm, 5 µm, Phenomenex Torrance, USA) and Shimadzu instrument (LC-10AVP Pump, UV-vis SDP-10AVP, Japan).…”

“…The amount of 1 ml of the external medium was withdrawn from the system at a predetermined time interval, replaced by an equal volume of fresh medium, and filtered through a 0.45-µm membrane. DFZ was assayed in the samples by liquid chromatography (LC) according to the methodology previously described, as mentioned in section 2.3.2 [21]. The diffusion of non-encapsulated form of DFZ across the dialysis bag was performed and used as control.…”

Response Surface Optimization of Ultra-Elastic Nanovesicles Loaded with Deflazacort Tailored for Transdermal Delivery: Accentuated Bioavailability and Anti-Inflammatory Efficacy

“…From the results obtained from clinical studies concerning evaluation of both therapeutic activity and safety of corticosteroid treatment, DFZ has favorable therapeutic and safety profiles compared to other corticosteroids. 5 , 6 Unfortunately, problems such as poor solubility, erratic absorption and many drug dosing are encountered with oral DFZ. 7 Additionally, gastrointestinal symptoms are the most frequently reported adverse events in DFZ recipient.…”

Deflazacort: therapeutic index, relative potency and equivalent doses versus other corticosteroids

“…Deflazacort has a smaller impact on calcium metabolism than any other synthetic corticosteroid, and therefore shows a lower risk of growth rate retardation in children [15, 16] and of osteoporosis in adult/elderly patients [2]. Another distinctive feature of deflazacort is its smaller influence on carbohydrate metabolism than other glucocorticoids, as demonstrated in both studies conducted on animal models [4] and in clinical trials [17, 18].…”

“…Deflazacort is a heterocyclic corticosteroid, oxazoline-derivative of prednisolone [2], characterized by high efficacy and good tolerability, as demonstrated by the results of several clinical studies that have evaluated its therapeutic activity and safety in conditions where corticosteroid treatment is indicated.…”