Hetero Drugs Ltd. (R&D), Plot No. B. 80 & 81, APIE, Balanagar, Hyderabad 500018, India.
J Pharm Biomed Anal. 2010 Mar 11;51(4):994-7. doi: 10.1016/j.jpba.2009.10.025. Epub 2009 Nov 6.
A stability-indicating gradient reverse phase liquid chromatographic purity and assay method for duloxetine hydrochloride (DUH) was developed and validated. DUH was subjected to the stress conditions and it is sensitive towards oxidative, acid and hydrolytic degradation. Successful separation of DUH from its two process impurities and one degradation impurity formed under stress conditions was achieved on a Symmetry C18, 250x4.6mm, 5microm column using a gradient mixture of solvent A (0.01M potassium dihydrogen orthophosphate having 0.2% triethyl amine, pH adjusted to 2.5 with orthophosphoric acid) and solvent B (20:80 v/v mixture of acetonitrile and methanol). The flow rate is 1ml/min and the detection wavelength is 230nm. The mass balance was found to be in the range of 99.2-99.7% in all the stressed conditions.
建立并验证了一种用于盐酸度洛西汀（DUH）的稳定性指示梯度反相高效液相色谱纯度和含量测定方法。DUH 经多种条件下的稳定性试验，结果表明其对氧化、酸和水解降解较为敏感。在 Symmetry C18，250x4.6mm，5μm 柱上，以溶剂 A（含 0.01M 磷酸二氢钾、0.2%三乙胺，用磷酸调 pH 至 2.5）和溶剂 B（乙腈和甲醇 20:80v/v 混合溶液）为梯度洗脱流动相，流速 1ml/min，检测波长 230nm，成功实现了 DUH 与其两种工艺杂质和一种降解产物在各种条件下的分离。在所有的稳定性条件下，其物料平衡均在 99.2-99.7%范围内。
