Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini Street, Giza 11562, Egypt.
J Anal Methods Chem. 2012;2012:754650. doi: 10.1155/2012/754650. Epub 2012 Feb 16.
Two simple, accurate, and sensitive methods were developed for the determination of netobimin in the presence of its degradation product. Method (A) was an HPLC method, performed on C18 column using acetonitrile/methanol/0.01 M potassium dihydrogen phosphate (56 : 14 : 30 by volume) as a mobile phase with a flow rate of 0.5 mL/min. Detection was performed at 254 nm. Method (B) was a TLC method, using silica gel 60 F(254) plates; the optimized mobile phase was toluene/methanol/chloroform/ammonium hydroxide (5 : 4 : 6 : 0.1 by volume). The spots were scanned densitometrically at 346 nm. Linearity ranges were 1-10 μg/mL for method (A) and 0.5-5 μg/band for method (B), and the mean percentage recoveries were 99.3 ± 0.7% and 99.7 ± 0.7% for methods (A) and (B), respectively. The proposed methods were found to be specific for netobimin in the presence of up to 90% of its degradation product. Statistical comparison between the results obtained by these methods and the manufacturer method was done, and no significance difference was obtained.
两种简单、准确且灵敏的方法被开发出来，用于在存在降解产物的情况下测定奈托比明。方法（A）是一种 HPLC 方法，在 C18 柱上进行，使用乙腈/甲醇/0.01 M 磷酸二氢钾（体积比为 56:14:30）作为流动相，流速为 0.5 mL/min。检测波长为 254nm。方法（B）是一种 TLC 方法，使用硅胶 60 F(254)板；优化的流动相为甲苯/甲醇/氯仿/氨水（体积比为 5:4:6:0.1）。斑点在 346nm 处进行扫描比色。方法（A）的线性范围为 1-10μg/mL，方法（B）的线性范围为 0.5-5μg/band，方法（A）和（B）的平均回收率分别为 99.3±0.7%和 99.7±0.7%。结果表明，在存在高达 90%降解产物的情况下，所提出的方法对奈托比明具有特异性。对这些方法和制造商方法获得的结果进行了统计学比较，没有发现显著差异。
