Trivedi Rakshit Kanubhai, Chendake Dhairyshil S, Patel Mukesh C
Analytical Research and Development, Integrated Product Development, Dr. Reddy's Laboratories Ltd., Bachupally, Hyderabad-500 072, India. ; P. S. Science and H. D. Patel Arts College, S. V. Campus, Kadi-382 715, Gujarat, India.
Sci Pharm. 2012 Jul-Sep;80(3):591-603. doi: 10.3797/scipharm.1204-06. Epub 2012 May 22.
A stability-indicating reversed-phase high performance liquid chromatography (RP-HPLC) method was developed for the simultaneous determination of Formoterol fumarate (FOR), Tiotropium bromide (TRI), and Ciclesonide (CLS) in a pulmonary drug product. The desired chromatographic separation was achieved on the Zorbax SB C8, 5 μm (150 × 4.6 mm) column, using gradient elution at 230 nm detector wavelength. The optimized mobile phase consisted of a 0.2 % v/v perchloric acid as solvent-A and acetonitrile as solvent-B. The developed method separated FOR, TRI, and CLS in the presence of its five unknown degradation products within 10 minutes. The stability-indicating capability was established by forced degradation experiments and the separation of unknown degradation products. The developed RP-HPLC method was validated according to the International Conference on Harmonization (ICH) guidelines. This validated method was applied for the simultaneous estimation of FOR, TRI, and CLS in commercially available Triohale(®) pMDI (Pressurized Metered-Dose Inhaler) samples. Furthermore, this method can be extended for individual estimation of FOR, TRI, and CLS in various commercially available pulmonary dosage forms.
建立了一种稳定性指示反相高效液相色谱（RP-HPLC）法，用于同时测定肺部药物制剂中富马酸福莫特罗（FOR）、噻托溴铵（TRI）和环索奈德（CLS）。在Zorbax SB C8，5μm（150×4.6mm）色谱柱上，于230nm检测波长下采用梯度洗脱实现了所需的色谱分离。优化后的流动相由0.2% v/v的高氯酸作为溶剂A和乙腈作为溶剂B组成。所建立的方法在10分钟内分离了FOR、TRI和CLS及其五种未知降解产物。通过强制降解实验和未知降解产物的分离确定了该方法的稳定性指示能力。所建立的RP-HPLC法根据国际协调会议（ICH）指南进行了验证。该验证方法用于同时测定市售Triohale(®) 压力定量吸入气雾剂（pMDI）样品中的FOR、TRI和CLS。此外，该方法可扩展用于各种市售肺部剂型中FOR、TRI和CLS的单独测定。
