Stability-Indicating RP-HPLC Method Development and Validation for Determination of Impurities in Loperamide Hydrochloride Capsules Dosage Form

IF 1.8 4区医学 Q4 BIOCHEMICAL RESEARCH METHODS

Biomedical Chromatography Pub Date : 2025-03-12 DOI:10.1002/bmc.70027

Sreenivas Pippalla, Vaishnavi Chintala

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引用次数: 0

Abstract

A quality by design (QbD)-based high-resolution, stability-indicating high-performance liquid chromatography (HPLC) method was developed for determining impurities in loperamide hydrochloride (LPH) tablet dosage forms. Using this method, eight known impurities were qualified, and three degradants were quantified with excellent peak resolution. Mobile Phase-A consisted of 0.05-M tetrabutylammonium hydrogen phosphate buffer and acetonitrile (80:20, v/v), while Mobile Phase-B contained the same buffer and acetonitrile (20:80, v/v). The gradient program was as follows: 0 min, MP-A 95%, MP-B 5%; 15 min, MP-A 30%, MP-B 70%; 17 min, MP-A 30%, MP-B 70%; 19 min, MP-A 95%, MP-B 5%; and 24 min, MP-A 95%, MP-B 5%. Chromatographic separation was performed using a column zodiac C18 (100 mm × 4.6 mm, 3.0 μm) with a flow rate of 1.5 mL/min, detection at 220 nm, an injection volume of 10 μL, and a column temperature of 35°C.

Stress studies revealed LPH's sensitivity to acidic, oxidative, and thermal conditions. Under all forced degradation conditions, the purity angle was found to be less than the purity threshold, demonstrating the robustness of the method. Validation confirmed its suitability for quality analysis and stability studies in routine manufacturing processes.

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为测定盐酸洛哌丁胺（LPH）片剂中的杂质，开发了一种基于质量设计（QbD）的高分辨率、稳定性指示高效液相色谱（HPLC）方法。利用该方法对 8 种已知杂质进行了定性，并对 3 种降解剂进行了定量，其峰分辨率极佳。流动相 A 由 0.05-M 磷酸氢四丁基铵缓冲液和乙腈（80:20, v/v）组成，流动相 B 由相同的缓冲液和乙腈（20:80, v/v）组成。梯度程序如下0 分钟，MP-A 95%，MP-B 5%；15 分钟，MP-A 30%，MP-B 70%；17 分钟，MP-A 30%，MP-B 70%；19 分钟，MP-A 95%，MP-B 5%；24 分钟，MP-A 95%，MP-B 5%。色谱分离使用的色谱柱为 zodiac C18（100 mm × 4.6 mm，3.0 μm），流速为 1.5 mL/min，检测波长为 220 nm，进样量为 10 μL，柱温为 35°C。应力研究表明，LPH 对酸性、氧化和热条件非常敏感。在所有强制降解条件下，纯度角都小于纯度阈值，这证明了该方法的稳健性。验证结果表明，该方法适用于常规生产过程中的质量分析和稳定性研究。

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

Biomedical Chromatography 生物-分析化学

CiteScore

3.60

自引率

5.60%

发文量

268

审稿时长

2.3 months

期刊介绍： Biomedical Chromatography is devoted to the publication of original papers on the applications of chromatography and allied techniques in the biological and medical sciences. Research papers and review articles cover the methods and techniques relevant to the separation, identification and determination of substances in biochemistry, biotechnology, molecular biology, cell biology, clinical chemistry, pharmacology and related disciplines. These include the analysis of body fluids, cells and tissues, purification of biologically important compounds, pharmaco-kinetics and sequencing methods using HPLC, GC, HPLC-MS, TLC, paper chromatography, affinity chromatography, gel filtration, electrophoresis and related techniques.