Katakam Lakshmi Narasimha Rao, Ettaboina Santhosh Kumar, Dongala Thirupathi
Department of Chemistry, JNTU Hyderabad, Hyderabad, India.
Quality Control, Aurex Laboratories LLC, East Windsor, New Jersey, USA.
Biomed Chromatogr. 2021 Oct;35(10):e5152. doi: 10.1002/bmc.5152. Epub 2021 May 17.
A stability-indicating HPLC method was developed for the simultaneous determination of paraben mixture and its degradation products in effervescent potassium chloride tablets. The chromatographic separation was achieved on a Waters Cortecs C18 column (2.7 μm, 4.6 × 150 mm) using gradient elution. The optimized mobile phase consisted of 0.1% orthophosphoric acid in purified water as solvent A and purified water, acetonitrile, and orthophosphoric acid (100:900:1, v/v) as solvent B. The flow rate was 0.8 mL/min, and column temperature was maintained at 35°C. The injection volume was 10 μL, and UV detection was carried out at 254 nm. The selectively developed method has optimal separation among p-hydroxybenzoic acid, methylparaben, ethylparaben, propylparaben, and butylparaben peaks in the presence of specified and unspecified degradation products in the determination of drug product. The mass balance obtained from forced degradation studies was ≥95% and thus proves the stability-indicating property of the developed method. The developed reversed-phase HPLC method has been validated according to the International Conference on Harmonization guidelines. The correlation coefficients for all the peaks were >0.9999. The results of the other validation parameters were found within the limits. Finally, the optimized method was used in the quality control lab for stability analysis.
建立了一种稳定性指示高效液相色谱法，用于同时测定泡腾氯化钾片中对羟基苯甲酸酯混合物及其降解产物。采用梯度洗脱，在Waters Cortecs C18柱（2.7μm，4.6×150mm）上实现色谱分离。优化后的流动相由0.1%正磷酸的纯化水作为溶剂A，以及纯化水、乙腈和正磷酸（100:900:1，v/v）作为溶剂B组成。流速为0.8mL/min，柱温保持在35°C。进样体积为10μL，在254nm处进行紫外检测。在药物产品测定中，该选择性开发的方法在存在特定和未指定降解产物的情况下，对羟基苯甲酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯峰之间具有最佳分离效果。强制降解研究得到的质量平衡≥95%，从而证明了所开发方法的稳定性指示特性。所开发的反相高效液相色谱法已根据国际协调会议指南进行了验证。所有峰的相关系数均>0.9999。其他验证参数的结果均在规定范围内。最后，优化后的方法用于质量控制实验室进行稳定性分析。
