Desmopressin acetate (DPA) is a synthetic analogue of vasopressin used in the treatment of diabetes insipidus, bedwetting, hemophilia A, and elevated levels of urea in the blood. Sensitive and selective stability-indicating methods are needed to be developed and validated for its assay pure and pharmaceutical dosage forms in the presence of its degradation products as no method has been reported for its determination in the presence of its degradants. This work describes a comparative study of five simple stability-indicating spectrophotometric techniques for determination of DPA in presence of its acid-degradation products (acid-degradants) without prior separation. The proposed spectrophotometric techniques (First derivative, Derivative ratio, Ratio difference, Mean centering and Dual wavelength) were developed and validated according to ICH guidelines. Acid degradation was carried out with 0.1 N HCl; the acid-degradants were separated on TLC plates and the acidic degradation pathway was established by IR, H-NMR and MS techniques. The TLC method was based on the separation of DPA and its acid-induced degradation products on silica gel plates using methanol: water (80:20, v/v) as a developing system and UV detection at 254 nm. All assay suggested methods were successfully applied for quantitation of DPA in pure and tablet forms. They are specific, sensitive, precise and accurate. They showed good linearity in the concentration range of 1–14 µg/mL with good correlation coefficients, and limit of detection (LOD) of 0.304, 0.274, 0.167, 0.248 and 0.199 and limit of quantitation (LOQ) of 0.920, 0.829, 0.506, 0.751 and 0.604) for each method, respectively. These methods were successfully applied for the simultaneous determination of DPA in its pure and tablet dosage form in the presence of its acid-degradants. The results obtained were statistically comparable with those of reported HPLC assay method; no significant differences were observed with relevance to accuracy and precision. All the methods are sensitive, selective and can be used for the routine analysis of DPA in its pure and dosage forms.
simple, rapid, sensitive, accurate and precise spectrophotometric stability-indicating methods were developed for the determination of dinitolimide in bulk powder and in pharmaceutical preparation. Method (A) First derivative (1D), Method (B) Ratio derivative (1DD), Method (C) Ratio difference (RD), Method (D) Bivariate and Method (E) Dual wavelength methods were used for the determination of intact dinitolimide in presence of its degradation product. These methods were validated and successfully applied to the determination of Zoamix ® 50mg powder with an average percent recovery { ± RSD% of 100.56 ± 1.280 for method (A), 100.07 ± 1.885 for method (B), 98.22 ± 1.414 for method (C), 99.96 ± 1.370 for method (D) and 99.05 ± 0.745 for method (E) and 98.75 ± 1.815 for method (F)}. The obtained results were statistically compared with those of the reported method by applying t-test and F-test at 95% confidence level and no significant difference was observed regarding accuracy and precision.
This study describes three spectrophotometric techniques that were developed and verified for the reliable identification of dalfampridine (DFP) in the presence of its oxidative derivative, namely (Derivative ratio 1DD, Ratio subtraction RD, and Bivariate BI); calibration graphs were established in the range of (1–14 ug/mL) with good correlation coefficients. The established techniques have been effectively used to analyze Dalfampridine (DFP) in its pharmaceutical dose form. The procedures were verified in accordance with ICH requirements, and accuracy, precision, and repeatability were determined to be satisfactory. The degradation pathway was confirmed using TLC, IR, 1H NMR and mass spectrometry. In addition to Analytical Greenness metrics (AGREE) method and Analytical Eco-Scale tools were applied for DFP with greenness assessment.
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