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TLC-spectrodensitometric method for simultaneous determination of dapagliflozin and rosuvastatin in rabbit plasma: stability indicating assay and kinetic studies.

ABSTRACT: Herein, a sensitive and reliable eco-friendly TLC-spectrodensitometric method has been established for the simultaneous determination of dapagliflozin (DAPA) and rosuvastatin (ROSV) for the first time. TLC separation was carried out on silica gel F₂₅₄ using ethyl acetate : methanol (5 : 0.1, v/v) as a mobile phase and UV measurement at 243 nm. The method was fully validated according to ICH guidelines. Acceptable separation was achieved with R _f values of 0.23 and 0.44 for DAPA and ROSV, respectively. Regression plots revealed linear relationships in the concentration range 20-2500 ng per band and 10-2500 ng per band with LODs of 6.60 and 3.57 ng per band for both DAPA and ROSV, respectively. The relative standard deviations (RSDs%) were found to be 1.35 and 0.53 for DAPA and ROSV, respectively. Moreover, kinetic studies were conducted for measurement of degradation rate constant (k) and half life time (t _1/2) of DAPA and ROSV via forced photo-degradation.

SUBMITTER: Abbas NS

PROVIDER: S-EPMC9057705 | biostudies-literature | 2020 Nov

REPOSITORIES: biostudies-literature

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TLC-spectrodensitometric method for simultaneous determination of dapagliflozin and rosuvastatin in rabbit plasma: stability indicating assay and kinetic studies.

Abbas Noha S NS Derayea Sayed M SM Omar Mahmoud A MA Saleh Gamal A GA

RSC advances 20201109 67

Herein, a sensitive and reliable eco-friendly TLC-spectrodensitometric method has been established for the simultaneous determination of dapagliflozin (DAPA) and rosuvastatin (ROSV) for the first time. TLC separation was carried out on silica gel F254 using ethyl acetate : methanol (5 : 0.1, v/v) as a mobile phase and UV measurement at 243 nm. The method was fully validated according to ICH guidelines. Acceptable separation was achieved with R f values of 0.23 and 0. ...[more]

PMID: 35519199

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Project description:BackgroundArtemisinin-based fixed dose combination (FDC) products are recommended by World Health Organization (WHO) as a first-line treatment. However, the current artemisinin FDC products, such as β-artemether and lumefantrine, are inherently unstable and require controlled distribution and storage conditions, which are not always available in resource-limited settings. Moreover, quality control is hampered by lack of suitable analytical methods. Thus, there is a need for a rapid and simple, but stability-indicating method for the simultaneous assay of β-artemether and lumefantrine FDC products.MethodsThree reversed-phase fused-core HPLC columns (Halo RP-Amide, Halo C18 and Halo Phenyl-hexyl), all thermostated at 30°C, were evaluated. β-Artemether and lumefantrine (unstressed and stressed), and reference-related impurities were injected and chromatographic parameters were assessed. Optimal chromatographic parameters were obtained using Halo RP-Amide column and an isocratic mobile phase composed of acetonitrile and 1 mM phosphate buffer pH 3.0 (52:48; V/V) at a flow of 1.0 ml/min and 3 μl injection volume. Quantification was performed at 210 nm and 335 nm for β-artemether and for lumefantrine, respectively. In-silico toxicological evaluation of the related impurities was made using Derek Nexus v2.0®.ResultsBoth β-artemether and lumefantrine were separated from each other as well as from the specified and unspecified related impurities including degradants. A complete chromatographic run only took four minutes. Evaluation of the method, including a Plackett-Burman robustness verification within analytical QbD-principles, and real-life samples showed the method is suitable for quantitative assay purposes of both active pharmaceutical ingredients, with a mean recovery relative standard deviation (± RSD) of 99.7 % (± 0.7%) for β-artemether and 99.7 % (± 0.6%) for lumefantrine. All identified β-artemether-related impurities were predicted in Derek Nexus v2.0® to have toxicity risks similar to β-artemether active pharmaceutical ingredient (API) itself.ConclusionsA rapid, robust, precise and accurate stability-indicating, quantitative fused-core isocratic HPLC method was developed for simultaneous assay of β-artemether and lumefantrine. This method can be applied in the routine regulatory quality control of FDC products. The in-silico toxicological investigation using Derek Nexus® indicated that the overall toxicity risk for β-artemether-related impurities is comparable to that of β-artemether API.

Dataset Information

TLC-spectrodensitometric method for simultaneous determination of dapagliflozin and rosuvastatin in rabbit plasma: stability indicating assay and kinetic studies.

Publications

TLC-spectrodensitometric method for simultaneous determination of dapagliflozin and rosuvastatin in rabbit plasma: stability indicating assay and kinetic studies.

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