Dongala Thirupathi, Katari Naresh Kumar, Palakurthi Ashok Kumar, Jonnalagadda Sreekantha B
Aurex Laboratories LLC, NJ, USA.
Department of Chemistry, GITAM deemed to be University, Hyderabad, Telangana, India.
Biomed Chromatogr. 2019 Oct;33(10):e4608. doi: 10.1002/bmc.4608. Epub 2019 Jun 27.
We developed novel stability-indicating HPLC method for simultaneous estimation of 14 impurities in excedrin tablet, a formulation with a combination of acetaminophen, aspirin, and caffeine. In addition, a new impurity that was generated through degradation of aspirin at high temperatures during the accelerated stability conditions was positively identified and confirmed, using liquid chromatography-mass spectrometry technique. The HPLC method was optimized using the Inertsustain C , 250 × 4.6 mm, 5.0 μm column, employing simple gradient method. Forced degradation studies were performed under acidic, basic, oxidative and thermal conditions to prove the scope and stability-indicating the nature of the method. The optimized method was validated as per the International Conference on Harmonization guidelines. The HPLC method showed linearity from LOQ concentration to 21 μg mL . Precision and intermediate precision values were <5% RSD. The validated HPLC method is currently applied for the routine testing of excedrin tablet formulations in quality control laboratories.
我们开发了一种新型的稳定性指示高效液相色谱法，用于同时测定复方阿司匹林片中的14种杂质，该制剂含有对乙酰氨基酚、阿司匹林和咖啡因。此外，利用液相色谱-质谱技术，成功鉴定并确认了一种在加速稳定性条件下高温时由阿司匹林降解产生的新杂质。该高效液相色谱法采用Inertsustain C 250×4.6 mm、5.0μm色谱柱，并采用简单梯度法进行了优化。在酸性、碱性、氧化和热条件下进行了强制降解研究，以证明该方法的适用范围和稳定性指示特性。该优化方法按照国际协调会议指南进行了验证。该高效液相色谱法在定量限浓度至21μg/mL范围内呈线性。精密度和中间精密度值的相对标准偏差（RSD）均<5%。经过验证的高效液相色谱法目前已应用于质量控制实验室对复方阿司匹林片制剂的常规检测。
