Prajapati Pintu, Ardeshana Princy, Kansara Yashwini, Shah Pranav, Pulusu Veera Shakar, Haque Anzarul, Kalam Mohd Abul, Shah Shailesh
Department of Quality Assurance and Department of Pharmaceutics, Maliba Pharmacy College, Maliba Campus, Bardoli-Mahuva Road, Tarsadi, Mahuva, Surat, 394 350, Gujarat, India.
Department of Quality Assurance and Department of Pharmaceutics, Maliba Pharmacy College, Maliba Campus, Bardoli-Mahuva Road, Tarsadi, Mahuva, Surat, 394 350, Gujarat, India.
Anal Biochem. 2025 May;700:115785. doi: 10.1016/j.ab.2025.115785. Epub 2025 Jan 30.
This study developed a microwave-aided spectrofluorimetric method for in-vivo characterizing teneligliptin-loaded solid dispersion adsorbate (TNG-SDA) using a quality by design approach. The microwave-aided chemical reaction was applied for derivatization of non-fluorescent teneligliptin with NBD-Cl (7-chloro-4-nitrobenzoxadiazole). TNG-SDA was prepared to enhance the solubility and bioavailability of teneligliptin, a BCS (Biopharmaceutical Classification System) class II drug. The method utilized environmentally friendly solvents and employed analytical quality by design principles for optimization. Critical method parameters were identified through failure mode impact analysis and optimized using response surface modelling. The fluorescence spectra of teneligliptin exhibited linearity across the concentration range of 50-250 ng/mL, with a correlation coefficient of 0.9978. The developed method was found to be accurate, precise, robust, specific and sensitive for estimation of teneligliptin. The method was applied to evaluate in vitro dissolution, pharmacokinetics, and pharmacodynamic of TNG-SDA compared to commercial formulations. Results showed significant improvements in teneligliptin solubility and bioavailability with the developed SDA. The microwave-aided derivatized fluorescent product was characterized by mass spectrometry. The method demonstrated environmental sustainability, robustness, sensitivity, cost-effectiveness, and user-friendliness when evaluated using white analytical chemistry approaches. It provided a sensitive and green alternative to existing hyphenated techniques for nanogram-level teneligliptin detection in pharmacokinetic studies.
本研究采用质量源于设计的方法，开发了一种微波辅助荧光光谱法，用于体内表征载有替格列汀的固体分散吸附物（TNG-SDA）。微波辅助化学反应用于用NBD-Cl（7-氯-4-硝基苯并恶二唑）对无荧光的替格列汀进行衍生化。制备TNG-SDA以提高替格列汀（一种BCS（生物药剂学分类系统）II类药物）的溶解度和生物利用度。该方法使用环境友好型溶剂，并采用质量源于设计的原则进行优化。通过失效模式影响分析确定关键方法参数，并使用响应面模型进行优化。替格列汀的荧光光谱在50-250 ng/mL浓度范围内呈线性，相关系数为0.9978。所开发的方法被发现对替格列汀的测定准确、精密、稳健、特异且灵敏。该方法用于评估TNG-SDA与市售制剂相比的体外溶出度、药代动力学和药效学。结果表明，所开发的SDA显著提高了替格列汀的溶解度和生物利用度。微波辅助衍生化荧光产物通过质谱进行表征。当使用白色分析化学方法进行评估时，该方法具有环境可持续性、稳健性、灵敏度、成本效益和用户友好性。它为药代动力学研究中纳克级替格列汀检测的现有联用技术提供了一种灵敏且绿色的替代方法。
