Pathak A, Rajput S J
Quality Assurance Laboratory, Centre of Relevance and Excellence in Novel Drug Delivery System, Pharmacy Department, G.H. Patel Building, Donor's Plaza, The Maharaja Sayajirao University of Baroda, Fatehgunj, Vadodara, Gujarat, India - 390 002.
J Chromatogr Sci. 2009 Aug;47(7):605-11. doi: 10.1093/chromsci/47.7.605.
A stability-indicating high-performance liquid chromatography method is developed for analysis of olanzapine and fluoxetine in the presence of their degradation products generated from forced decomposition studies as prescribed by the International Conference on Harmonization. Hydrolysis, oxidation, photolysis, and thermal degradation are evaluated by subjecting the drug substances to stress conditions. Successful separation of drugs from degradation products is achieved on a reversed-phase C(18) column using 75 mM potassium dihydrogen phosphate buffer (pH 4.0)-acetonitrile-methanol (55:40:5, v/v/v) as the mobile phase. The flow rate is 0.8 mL/min, and the detection wavelength is 227 nm. The method is validated with respect to linearity, precision, accuracy, system suitability, and robustness. The utility of the procedure is verified by its application to marketed formulations that are subjected to accelerated stability studies. Good separation of the drugs and their degradation products is observed using this method. The products formed in marketed tablet dosage forms are similar to those formed in standard drug solutions under similar stress conditions.
按照国际协调会议规定的强制降解研究，开发了一种稳定性指示高效液相色谱法，用于分析奥氮平和氟西汀及其降解产物。通过将原料药置于胁迫条件下，评估水解、氧化、光解和热降解情况。在反相C(18)柱上，以75 mM磷酸二氢钾缓冲液（pH 4.0）-乙腈-甲醇（55:40:5，v/v/v）为流动相，成功实现了药物与降解产物的分离。流速为0.8 mL/min，检测波长为227 nm。该方法在线性、精密度、准确度、系统适用性和稳健性方面得到了验证。通过将该方法应用于进行加速稳定性研究的市售制剂，验证了该程序的实用性。使用该方法观察到药物及其降解产物的良好分离。市售片剂剂型中形成的产物与在类似胁迫条件下标准药物溶液中形成的产物相似。
