Kowtharapu Leela Prasad, Katari Naresh Kumar, Ch Surekha, Sandoval Christian A, Muchakayala Siva Krishna, Konduru Naresh
Analytical Development Department, Shenzhen DEC Pharmaceutical Co., Ltd, Shenzhen, China.
Department of Chemistry, School of Science, GITAM (Deemed to be University), Hyderabad, India.
Biomed Chromatogr. 2022 Jun;36(6):e5359. doi: 10.1002/bmc.5359. Epub 2022 Mar 15.
Mast cell stabilizer and histamine receptor antagonist olopatadine hydrochloride (OPT) assay method predicated on LC have been established for the analysis in multiple formulations. The current method dealt with ophthalmic solution, nasal spray, and tablet formulation products. The isocratic chromatography method was optimized and validated with a Boston green C8 column (150 × 4.6 mm, 5 μm i.d.). Sodium dihydrogen phosphate buffer (pH 3.5) with acetonitrile in the ratio of 75:25 (v/v) was used as a mobile phase at a flow rate of 1.0 mL min and at the column temperature of 30°C, and the detection was done at 299 nm. The method was validated as per International Council for Harmonisation (ICH) guidelines and United States Pharmacopoeia (USP). The accuracy results ranged from 99.9 to 100.7%, % relative standard deviation (RSD) from the precision was 0.5, and correlation coefficient from the linearity experiment was > 0.999. Solution stability was established for 24 h at room temperature and refrigerator conditions, and it was found that the solutions were stable. Using quality by design-based experiment designs, critical quality attributes were studied and it was found that the method was robust. In all the forced degradation studies peak purity was passed, and no interference was found at the retention time of the active component. The method validation data demonstrated that the developed method is linear, precise, accurate, specific, robust, and stable for the determination of OPT from multiple formulations. Analytical eco-scale tool, Green Analytical Procedure Index (GAPI) tool, and the National Environmental Method Index (NEMI) were used to evaluate the greenness of the method, and the analytical eco-score of 77 for the presented method was found to be excellent.
已建立基于液相色谱法（LC）的肥大细胞稳定剂和组胺受体拮抗剂盐酸奥洛他定（OPT）分析方法，用于多种制剂的分析。当前方法适用于眼药水、鼻喷雾剂和片剂制剂产品。采用等度色谱法，使用波士顿绿C8柱（150×4.6 mm，内径5μm）进行优化和验证。以磷酸二氢钠缓冲液（pH 3.5）与乙腈按75:25（v/v）的比例作为流动相，流速为1.0 mL/min，柱温为30°C，检测波长为299 nm。该方法按照国际协调理事会（ICH）指南和美国药典（USP）进行验证。准确度结果在99.9%至100.7%之间，精密度的相对标准偏差（RSD）为0.5%，线性实验的相关系数>0.999。在室温和冷藏条件下确定溶液稳定性为24小时，发现溶液稳定。采用基于质量源于设计的实验设计，研究关键质量属性，发现该方法具有稳健性。在所有强制降解研究中，峰纯度均通过，在活性成分保留时间处未发现干扰。方法验证数据表明，所开发的方法对于多种制剂中OPT的测定具有线性、精密、准确、特异、稳健和稳定的特点。使用分析生态规模工具、绿色分析程序指数（GAPI）工具和国家环境方法指数（NEMI）来评估该方法的绿色度，发现所提出方法的分析生态评分为77，非常出色。
