Analytical Chemistry Department, Faculty of Pharmacy, Beni-Suef University, Egypt.
Talanta. 2010 Mar 15;80(5):2007-15. doi: 10.1016/j.talanta.2009.11.002. Epub 2009 Nov 10.
Simple, accurate, sensitive and validated UV spectrophotometric, chemometric and HPTLC-densitometric methods were developed for determination of oxybutynin hydrochloride (OX) in presence of its degradation product and additives in its pharmaceutical formulations. Method A is the first derivative of ratio spectra (DD(1)) which allows the determination of OX in presence of its degradate in pure form and tablets by measuring the peaks amplitude at 216 nm. Method B and C are principal component regression (PCR) and partial least-squares (PLS) for determination of OX in presence of its degradate in pure form, tablets and syrup. While, the developed high performance thin layer chromatography HPTLC-densitometric method was based on the separation of OX from its degradation product, methylparaben and propylparaben followed by densitometric measurement at 220 nm which allows the determination of OX in pure form, tablets and syrup. The separation was achieved using HPTLC silica gel F(254) plates and chloroform:methanol:ammonia solution:triethylamine (100:3:0.5:0.2, v/v/v/v) as the developing system. The accuracy, precision and linearity ranges of the developed methods were determined. The results obtained were statistically compared with each other and to that of a reported HPLC method, and there was no significant difference between the proposed methods and the reported method regarding both accuracy and precision.
建立了简单、准确、灵敏的紫外分光光度法、化学计量学和 HPTLC 分光光度法，用于在其制剂中存在降解产物和添加剂的情况下测定盐酸奥昔布宁（OX）。方法 A 是比值光谱的一阶导数（DD(1)），允许在纯形式和片剂中存在其降解产物的情况下测定 OX，通过测量 216nm 处的峰振幅。方法 B 和 C 是主成分回归（PCR）和偏最小二乘法（PLS），用于在纯形式、片剂和糖浆中存在其降解产物的情况下测定 OX。同时，所开发的高效薄层色谱 HPTLC 分光光度法基于 OX 与其降解产物、甲基对羟基苯甲酸甲酯和对羟基苯甲酸丙酯的分离，然后在 220nm 处进行分光光度测量，允许在纯形式、片剂和糖浆中测定 OX。分离是在 HPTLC 硅胶 F(254)板上，使用氯仿：甲醇：氨溶液：三乙胺（100:3:0.5:0.2，v/v/v/v）作为展开系统进行的。确定了所开发方法的准确性、精密度和线性范围。所得结果相互之间以及与报道的 HPLC 方法进行了统计学比较，并且在所提出的方法和报道的方法之间，在准确性和精密度方面均没有显著差异。
