Satínský Dalibor, Huclová Jitka, Solich Petr, Karlícek Rolf
The Research Centre LN00B125, Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Heyrovského 1203, Hradec Králové 500 05, Czech Republic.
J Chromatogr A. 2003 Oct 10;1015(1-2):239-44. doi: 10.1016/s0021-9673(03)01239-1.
A commercially available porous silica rod column was used as a separation tool for the sequential injection analysis (SIA). A porous solid monolithic column showed high performance at a low pressure, allowing sequential injection analysis to be used for the first time for separation in HPLC fashion. In this contribution, we tried to demonstrate a new separation concept with SIA manifold for the simultaneous determination of four different compounds (methylparaben (MP), propylparaben (PP), triamcinolone acetonide (TCA) and internal standard ketoprofen (KP)) in a pharmaceutical triamcinolon cream 0.1% formulation. A Chromolith Flash RP-18e, 25 mm x 4.6 mm column with a 10 mm pre-column (Merck, Germany) and a FIAlab 3000 system (USA) with an 8-port selection valve and 10 ml syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile-methanol-water (35:5:65, v/v/v) + 0.05% nonylamine, pH 2.5, flow rate 0.6 ml min(-1). The analysis time was <6 min. A novel sequential injection chromatography (SIC) technique with UV spectrophotometric detection was optimised and validated.
使用市售的多孔硅胶柱作为顺序注射分析（SIA）的分离工具。多孔整体柱在低压下表现出高性能，首次使顺序注射分析能够以高效液相色谱（HPLC）方式用于分离。在本论文中，我们尝试展示一种使用SIA流路的新分离概念，用于同时测定0.1%曲安奈德乳膏制剂中的四种不同化合物（对羟基苯甲酸甲酯（MP）、对羟基苯甲酸丙酯（PP）、曲安奈德（TCA）和内标酮洛芬（KP））。在我们的研究中，使用了一根Chromolith Flash RP - 18e，25 mm×4.6 mm柱，带有10 mm的预柱（德国默克公司），以及一台带有8通选择阀和10 ml注射器的FIAlab 3000系统（美国）进行顺序注射色谱分离。所用流动相为乙腈 - 甲醇 - 水（35:5:65，v/v/v） + 0.05%壬胺，pH 2.5，流速0.6 ml min⁻¹。分析时间<6分钟。优化并验证了一种采用紫外分光光度检测的新型顺序注射色谱（SIC）技术。
