Zawilla N H, Diana J, Hoogmartens J, Adams E
National Organization for Drug Control and Research, Cairo, Egypt.
J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Apr 3;833(2):191-8. doi: 10.1016/j.jchromb.2006.01.034. Epub 2006 Feb 28.
An isocratic liquid chromatographic method with pulsed electrochemical detection is described for the determination of neomycin in the presence of its impurities. The mobile phase is composed of an aqueous solution containing 35 g/l of sodium sulphate, 1 g/l of sodium 1-octanesulfonate, 14 ml/l of tetrahydrofuran (THF) and 50 ml/l of 0.2 M phosphate buffer pH 3.0. Sodium hydroxide was added post column to enhance the detection. An investigation of different reversed-phase columns indicated that the Discovery (C18 5 microm, 250 mm x 4.6 mm I.D.) column was the most suitable. The proposed method shows high efficiency, allowing the separation of the main component neomycin B from neomycin C and 15 other impurities. A central composite design was used to assess the robustness of the method. The method showed good selectivity, repeatability, linearity and sensitivity. This method was applied to analyse commercial samples.
描述了一种采用脉冲电化学检测的等度液相色谱法，用于在杂质存在的情况下测定新霉素。流动相由含有35 g/l硫酸钠、1 g/l 1-辛烷磺酸钠、14 ml/l四氢呋喃（THF）和50 ml/l 0.2 M pH 3.0磷酸盐缓冲液的水溶液组成。柱后添加氢氧化钠以增强检测效果。对不同反相柱的研究表明，Discovery（C18 5微米，250 mm×4.6 mm内径）柱最为合适。所提出的方法显示出高效率，能够将主要成分新霉素B与新霉素C及其他15种杂质分离。采用中心复合设计来评估该方法的稳健性。该方法具有良好的选择性、重复性、线性和灵敏度。该方法应用于商业样品的分析。
