新型 RP-HPLC 法同时测定片剂中的达帕格列净和替尼列汀,并通过 LC-MS/MS 鉴定降解产物

IF 3.4 Q2 PHARMACOLOGY & PHARMACY
Thummar Kashyap, Kevat Honey, Vadher Priyanka, Jesur Mihir
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引用次数: 0

摘要

背景全球有数百万人患有糖尿病,需要采取有效的管理策略。为满足这一需求,格兰马克制药有限公司于 2022 年推出了泰利列汀和达帕格列净的固定剂量复方制剂。结果 建立了一种同时测定药物制剂中达帕格列汀和替格列汀稳定性的 RP-HPLC 方法。采用 Zorbax Eclipse Plus C18 色谱柱(150 mm × 4.6 mm, 5 µm)进行分离。流动相由 10 mM 水乙酸铵缓冲液、甲醇和乙腈按适当比例混合而成,流速为 0.6 mL/min。使用光电二极管阵列 (PDA) 检测器在 224 纳米波长下检测等度洗脱液。根据 ICH 指南对各种应力条件进行的验证显示,主要在酸性、碱性和氧化应力条件下,替格列汀会发生明显降解。此外,还对在酸性、碱性和氧化条件下生成的替格列汀主要降解产物进行了基于液相色谱串联质谱(LC-MS/MS)的表征。 结论所开发的 RP-HPLC 方法采用稳定性指示方法,为同时测定药物制剂中的达帕格列净和替格列汀提供了一种有效方法。该方法在各种应力条件下均观察到明显的降解现象,并成功地分离了降解产物。所提出的方法直接用于降解产物的表征,根据 LC-MS/MS 数据生成了降解产物的结构,并预测了各种应力条件下的降解途径。所提出的方法确保了制药行业质量控制过程中结果的准确性和精确性,并且符合 ICH 验证指南的要求,证实了其在评估这些化合物稳定性方面的可靠性。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Novel RP-HPLC method for simultaneous determination of dapagliflozin and teneligliptin in tablet formulation and identification of degradation products by LC-MS/MS

Background

Diabetes mellitus affects millions globally, necessitating effective management strategies. Glenmark Pharmaceutical Limited introduced a fixed-dose combination of teneligliptin and dapagliflozin in 2022 to address this need. However, existing methods for their simultaneous detection are limited, lacking forced degradation studies essential for assessing drug stability.

Results

A stability-indicating RP-HPLC method was developed for the simultaneous determination of dapagliflozin and teneligliptin in pharmaceutical formulations. The separation was efficiently achieved employing a Zorbax Eclipse Plus C18 column (150 mm × 4.6 mm, 5 µm). The mobile phase comprised a mixture of 10 mM ammonium acetate buffer in water, methanol, and acetonitrile in a suitable proportion and delivered at a flow rate of 0.6 mL/min. Detection of the isocratic eluents was performed at 224 nm using a photodiode array (PDA) detector. Validation against various stress conditions, as per ICH guidelines, revealed significant degradation of teneligliptin primarily under acidic, basic, and oxidative stress. Moreover, liquid chromatography tandem mass spectrometry (LC-MS/MS)-based characterization was conducted for the primary degradation products of teneligliptin generated under acidic, basic, and oxidative conditions.

Conclusions

The developed RP-HPLC method with a stability-indicating approach provides an efficient means for the simultaneous determination of dapagliflozin and teneligliptin in pharmaceutical formulations. The significant degradation was observed under various stress conditions and also successfully separated the degradation products by this method. The proposed method directly applied for the characterization of degradation products and based on LC-MS/MS data the structure of degradation products was generated and also degradation pathways under various stress conditions were predicted. The proposed method ensured accurate and precise results in quality control process in pharmaceutical industry, and adherence to ICH validation guidelines affirms its reliability in assessing the stability of these compounds.

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来源期刊
自引率
0.00%
发文量
44
审稿时长
23 weeks
期刊介绍: Future Journal of Pharmaceutical Sciences (FJPS) is the official journal of the Future University in Egypt. It is a peer-reviewed, open access journal which publishes original research articles, review articles and case studies on all aspects of pharmaceutical sciences and technologies, pharmacy practice and related clinical aspects, and pharmacy education. The journal publishes articles covering developments in drug absorption and metabolism, pharmacokinetics and dynamics, drug delivery systems, drug targeting and nano-technology. It also covers development of new systems, methods and techniques in pharmacy education and practice. The scope of the journal also extends to cover advancements in toxicology, cell and molecular biology, biomedical research, clinical and pharmaceutical microbiology, pharmaceutical biotechnology, medicinal chemistry, phytochemistry and nutraceuticals.
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