Havlíková L, Matysová L, Nováková L, Solich P
Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Heyrovského 1203, 500 05 Hradec Králové, Czech Republic.
J Pharm Biomed Anal. 2006 May 3;41(2):671-5. doi: 10.1016/j.jpba.2006.01.012. Epub 2006 Feb 13.
A RP-HPLC method for simultaneous determination of calcium pantothenate and two preservatives methylparaben and propylparaben present in topical cream was developed. Different analytical columns with various stationary phases were tested. During method development, Supelco Discovery C18 column (125 mmx4.0 mm, 5 microm) and Zorbax SB-CN column (150 mmx4.6 mm, 5 microm) were tested. Both were not convenient for analytical separation because of the co-elution of calcium pantothenate with dead volume, and problems with the peak-shape of all components. Good separation was achieved using Zorbax TSM (250 mmx4.6 mm, 5 microm) and Hypersil ODS column (250 mmx4.6 mm, 5 microm), the latter was finally used for the analysis. The analysis time was 12 min, at flow rate 0.7 ml min-1. Chromatography was performed using binary mobile phase composed of methanol and phosphoric acid, pH 2.5, 65:35 (v/v). UV detection was accomplished at 214 nm. The method was validated according to ICH guideline recommendations. The method is suitable for practical routine analysis of commercially produced topical pharmaceutical preparations.
建立了一种反相高效液相色谱法，用于同时测定局部乳膏中泛酸钙以及两种防腐剂对羟基苯甲酸甲酯和对羟基苯甲酸丙酯的含量。对具有不同固定相的不同分析柱进行了测试。在方法开发过程中，测试了Supelco Discovery C18柱（125 mm×4.0 mm，5 µm）和Zorbax SB-CN柱（150 mm×4.6 mm，5 µm）。由于泛酸钙与死体积共洗脱以及所有组分峰形存在问题，这两种柱都不便于进行分析分离。使用Zorbax TSM柱（250 mm×4.6 mm，5 µm）和Hypersil ODS柱（250 mm×4.6 mm，5 µm）实现了良好的分离，最终使用后者进行分析。分析时间为12分钟，流速为0.7 ml min-1。使用由甲醇和pH 2.5的磷酸组成的二元流动相（65:35，v/v）进行色谱分析。在214 nm处进行紫外检测。该方法根据国际人用药品注册技术协调会（ICH）指南建议进行了验证。该方法适用于市售局部药物制剂的实际常规分析。
Zotero 插件