Development and Validation of Robust, Highly Sensitive and Stability-Indicating RP-HPLC Method for Estimation of Deferasirox and its Degradation Products.

IF 1.5 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS Journal of chromatographic science Pub Date : 2024-10-01 DOI:10.1093/chromsci/bmad032

Tarun Shishodia, Parul Grover, K Nagarajan, Monika Bhardwaj, Bhawna Chopra

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Abstract

A rapid, simple and highly sensitive stability-indicating reverse-phase high-performance liquid chromatographic technique, coupled with a photodiode array detector, was developed and validated for the estimation of Deferasirox (DFS). The chromatographic separation was achieved using a C-18 (250 × 4.6 mm, 5 μm) stationary phase and a mobile phase composed of 0.1% orthophosphoric acid and acetonitrile at a flow rate of 1 mL/min. The detection was carried out at a wavelength of 245 nm with a constant injection volume of 10 μL throughout the analysis. With an R2 value of 0.9996, the calibration curve was determined to be linear over an appropriate concentration range of 50-500 ng/mL. According to the International Conference on Harmonization (ICH) Q1 (R2) guideline, DFS was evaluated under stress conditions that included hydrolytic (acid, alkali and neutral), oxidative and thermal degradation. The findings demonstrated that significant degradation was observed in acidic degradation conditions, whereas drug substance was found to be stable when exposed to neutral, basic, oxidative and thermal degradation. The developed method was validated as per ICH guidelines. The developed method was employed successfully to estimate the amount of DFS in bulk and pharmaceutical formulation.

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开发并验证用于估算地拉羅司及其降解产物的稳健、高灵敏度和稳定性指示的 RP-HPLC 方法。

开发并验证了一种快速、简便、高灵敏度的稳定性指示反相高效液相色谱技术，该技术与光电二极管阵列检测器联用，可用于地拉罗司（DFS）的测定。色谱分离采用 C-18 (250 × 4.6 mm, 5 μm)固定相和由 0.1% 正磷酸和乙腈组成的流动相，流速为 1 mL/min。检测波长为 245 nm，整个分析过程的进样量保持为 10 μL。校准曲线的 R2 值为 0.9996，在 50-500 纳克/毫升的适当浓度范围内线性良好。根据国际协调会议（ICH）Q1 (R2)指南，在包括水解（酸、碱和中性）、氧化和热降解在内的压力条件下对 DFS 进行了评估。结果表明，在酸性降解条件下观察到了明显的降解，而在中性、碱性、氧化和热降解条件下发现药物是稳定的。根据 ICH 指南对所开发的方法进行了验证。所开发的方法成功地用于估算散装和药物制剂中 DFS 的含量。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Journal of chromatographic science 化学-分析化学

CiteScore

2.90

自引率

7.70%

发文量

审稿时长

5.6 months

期刊介绍： The Journal of Chromatographic Science is devoted to the dissemination of information concerning all methods of chromatographic analysis. The standard manuscript is a description of recent original research that covers any or all phases of a specific separation problem, principle, or method. Manuscripts which have a high degree of novelty and fundamental significance to the field of separation science are particularly encouraged. It is expected the authors will clearly state in the Introduction how their method compares in some markedly new and improved way to previous published related methods. Analytical performance characteristics of new methods including sensitivity, tested limits of detection or quantification, accuracy, precision, and specificity should be provided. Manuscripts which describe a straightforward extension of a known analytical method or an application to a previously analyzed and/or uncomplicated sample matrix will not normally be reviewed favorably. Manuscripts in which mass spectrometry is the dominant analytical method and chromatography is of marked secondary importance may be declined.