Chhalotiya Usmangani K, Bhatt Kashyap K, Shah Dimal A, Baldania Sunil L
Indukaka Ipcowala College of Pharmacy, Beyond GIDC Phase IV, Vithal Udyognagar, New Vallabh Vidyanagar-388121, Anand, Gujarat, India.
Sci Pharm. 2010 Oct-Dec;78(4):857-68. doi: 10.3797/scipharm.1009-11. Epub 2010 Oct 25.
The objective of the present work was to develop a stability-indicating RP-HPLC method for duloxetine hydrochloride (DUL) in the presence of its degradation products generated from forced decomposition studies. The drug substance was found to be susceptible to stress conditions of acid hydrolysis. The drug was found to be stable to dry heat, photodegradation, oxidation and basic condition attempted. Successful separation of the drug from the degradation products formed under acidic stress conditions was achieved on a Hypersil C-18 column (250 mm à 4.6 mm id, 5Îm particle size) using acetonitrile: 0.01 M potassium dihydrogen phosphate buffer (pH 5.4 adjusted with orthophosphoric acid) (50:50, v/v) as the mobile phase at a flow rate of 1.0 ml/min. Quantification was achieved with photodiode array detection at 229 nm over the concentration range 1â25 Îg/ml with range of recovery 99.8â101.3 % for DUL by the RP-HPLC method. Statistical analysis proved the method to be repeatable, specific, and accurate for estimation of DUL. It can be used as a stability-indicating method due to its effective separation of the drug from its degradation products.
本研究的目的是开发一种稳定性指示反相高效液相色谱法，用于测定盐酸度洛西汀（DUL）及其在强制降解研究中产生的降解产物。结果发现，该原料药易受酸水解的应激条件影响。该药物在尝试的干热、光降解、氧化和碱性条件下是稳定的。使用Hypersil C-18柱（250 mm×4.6 mm内径，5μm粒径），以乙腈：0.01 M磷酸二氢钾缓冲液（用正磷酸调节pH值至5.4）（50:50，v/v）作为流动相，流速为1.0 ml/min，成功实现了药物与酸性应激条件下形成的降解产物的分离。通过反相高效液相色谱法，在229 nm处采用光电二极管阵列检测，在1-25μg/ml的浓度范围内进行定量，DUL的回收率为99.8-101.3%。统计分析证明该方法对于DUL的测定具有可重复性、特异性和准确性。由于其能有效分离药物及其降解产物，该方法可作为一种稳定性指示方法。
