Comprehensive analysis of Aspirin and Apixaban: thedevelopment, validation, and forced degradation studies of bulk drugs and in-house capsule formulations using the RP-HPLC method.

IF 1.7 4区医学 Q3 MEDICINE, RESEARCH & EXPERIMENTAL

American journal of translational research Pub Date : 2024-10-15 eCollection Date: 2024-01-01 DOI:10.62347/VYDX5901

Tarang Patel, Mehul Patel, Umang Shah, Ashish Patel, Swayamprakash Patel, Nilay Solanki, Siddharth Shah

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引用次数: 0

Abstract

Objectives: This study aimed to develop a robust Reverse Phase-High-Performance Liquid Chromatography (RP-HPLC) method for simultaneous determination of Aspirin (ASP) and Apixaban (API) in bulk and in-house capsule formulations.

Methods: The separation was conducted on a Phenomenex Luna C₁₈ column using a Shimadzu LC20AT High-performance liquid chromatography (HPLC) system. The mobile phase consisted of 40:60 Acetonitrile (ACN): phosphate buffer (pH 4) modified by O-Phosphoric Acid (OPA). The parameters included a flow rate of 1 ml/min, a column temperature of 30°C, and Ultra-Violet (UV) detection at 227 nm. Method validation encompassed linearity, precision (Intraday and Interday), accuracy (% Recovery), and sensitivity (Limit of Detection (LOD) and Limit of Quantification (LOQ)). Stability testing followed The International Council for Harmonization (ICH) guidelines.

Results: The developed method demonstrated reliable separation of Aspirin and Apixaban with retention times of 5.37 min and 7.10 min, respectively. It exhibited linearity over the concentration ranges of 50-300 μg/mL for Aspirin and 5-15 μg/mL for Apixaban. The recovery percentage ranged from 90.02% to 101% for Aspirin and 98.18% to 101.18% for Apixaban. LOD and LOQ were determined as 0.84 μg/mL and 2.55 μg/mL for Aspirin, and 0.41 μg/mL and 1.24 μg/mL for Apixaban, respectively. Stability testing confirmed the method's robustness under various stress conditions.

Conclusions: The validated RP-HPLC method offers a reliable tool for routine analysis of Aspirin and Apixaban in pharmaceutical formulations, highlighting its potential for combined dosage applications and routine quality control.

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阿司匹林和阿哌沙班的综合分析：使用 RP-HPLC 方法对散装药物和内部胶囊制剂进行开发、验证和强制降解研究。

研究目的本研究旨在开发一种稳健的反相高效液相色谱（RP-HPLC）方法，用于同时测定散装和内部胶囊制剂中的阿司匹林（ASP）和阿哌沙班（API）：采用岛津 LC20AT 高效液相色谱（HPLC）系统，在 Phenomenex Luna C18 色谱柱上进行分离。流动相为 40:60 乙腈（ACN）：经 O-磷酸（OPA）改良的磷酸盐缓冲液（pH 4）。参数包括流速 1 ml/min、柱温 30°C、紫外检测波长 227 nm。方法验证包括线性、精确度（日内和日间）、准确度（回收率%）和灵敏度（检测限（LOD）和定量限（LOQ））。稳定性测试遵循了国际协调理事会（ICH）的指导原则：所开发的方法可靠地分离了阿司匹林和阿哌沙班，保留时间分别为 5.37 分钟和 7.10 分钟。阿司匹林和阿哌沙班在 50-300 μg/mL 和 5-15 μg/mL 的浓度范围内呈线性关系。阿司匹林的回收率为 90.02% 至 101%，阿哌沙班的回收率为 98.18% 至 101.18%。阿司匹林的最低检出限（LOD）和最低定量限（LOQ）分别为0.84 μg/mL和2.55 μg/mL，阿哌沙班的最低检出限（LOD）和最低定量限（LOQ）分别为0.41 μg/mL和1.24 μg/mL。稳定性测试证实了该方法在各种压力条件下的稳健性：经过验证的 RP-HPLC 方法为药物制剂中阿司匹林和阿哌沙班的常规分析提供了可靠的工具，凸显了其在复合制剂应用和常规质量控制方面的潜力。

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来源期刊

American journal of translational research ONCOLOGY-MEDICINE, RESEARCH & EXPERIMENTAL

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552

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