Bandaru Lova Gani Raju, Konduru Naresh, Kowtharapu Leela Prasad, Gundla Rambabu, Kanuparthy Phani Raja, Katari Naresh Kumar
Department of Chemistry, GITAM School of Science, GITAM Deemed to Be University, Hyderabad, India.
Biomed Chromatogr. 2025 Feb;39(2):e6062. doi: 10.1002/bmc.6062.
A simple LC method has been developed and validated for estimating budesonide (epimer B + A) and formoterol fumarate dihydrate in dry powder inhalation. The development results of this study make it very significant. The degradation and process impurities in EP and ChP were identified in addition to budesonide and formoterol fumarate. As of yet, no one has reported all impurities using a single method. It is a unique research because it analyzes APSD (Aerodynamic Particle Size Distribution), DDU (Delivered Dose Uniformity), BU (Blend Uniformity), Assay, and cleaning test samples. It enhances the quality of medicine and separates all organic impurities and isomers through a suitable stationary phase (YMC-Pack Pro C18, 150 × 4.6 mm × 3 μm). We optimized the chromatographic conditions: Injection volume was 20 μL, and flow rate was 1.0 mL/min. The wavelength was optimized at 220 nm. After experimental and validation results. An example is A, which contains sodium dihydrogen orthophosphate monohydrate, sodium 1-decane sulfonate, adjusted pH 3.0, and acetonitrile at a ratio of 80:20 (v/v), and B, which contains pH 3.0 buffer and acetonitrile at a ratio of 20:80 (v/v) respectively. In addition to being optimized, the test method was validated according to ICH Q2(R2).
已开发并验证了一种简单的液相色谱法,用于测定干粉吸入剂中的布地奈德(差向异构体B + A)和富马酸福莫特罗二水合物。本研究的开发结果具有重要意义。除了布地奈德和富马酸福莫特罗外,还鉴定了欧洲药典和中国药典中的降解产物和工艺杂质。迄今为止,尚未有人用单一方法报道所有杂质。这是一项独特的研究,因为它分析了空气动力学粒径分布(APSD)、递送剂量均匀性(DDU)、混合均匀性(BU)、含量测定以及清洁测试样品。它提高了药品质量,并通过合适的固定相(YMC-Pack Pro C18,150×4.6 mm×3μm)分离所有有机杂质和异构体。我们优化了色谱条件:进样体积为20μL,流速为1.0 mL/min。波长优化为220 nm。经过实验和验证结果。例如,流动相A含有一水合磷酸二氢钠、1-癸烷磺酸钠,pH值调至3.0,乙腈比例为80:20(v/v),流动相B含有pH值为3.0的缓冲液和乙腈,比例分别为20:80(v/v)。除了进行优化外,该测试方法还根据ICH Q2(R2)进行了验证。