De Rossi Antonella, Desiderio Claudia
Institute of Chemical Methodology, National Council of Research, Rome Research Area, Monterotondo Scalo, Rome, Italy.
Electrophoresis. 2002 Sep;23(19):3410-7. doi: 10.1002/1522-2683(200210)23:19<3410::AID-ELPS3410>3.0.CO;2-I.
A fast capillary electrochromatographic method was developed for the analysis of paraben preservatives in drugs and cosmetics in the presence of their main metabolite and/or impurity, 4-hydroxybenzoic acid. The separation was optimized in a 75 num ID capillary, fully packed with 5 num C18 stationary phase, studying the effects of mobile phase pH and composition (buffer type and organic solvent content). The mobile phase 5 mM ammonium formate, pH 3.0, containing 65% acetonitrile allowed us to obtain the baseline separation of methyl-, ethyl-, propyl-, butyl-, and benzylparabens from a mixture in less than 2.5 min with repeatability and linearity using the short-end injection method (8 cm separation capillary effective length). Under the optimum experimental conditions, the method provided high separation efficiency for parabens, in the range of 129 312-140 325 number of theoretical plates per meter, and analyte quantitation limits (LOQs) in the range of 1.25-2.50 nug/mL. The method was successfully applied to the quantitative analysis of paraben preservatives in pharmaceutical and cosmetic industrial samples with direct injection or after reduced sample pretreatment.
建立了一种快速毛细管电色谱法,用于分析药物和化妆品中的对羟基苯甲酸酯类防腐剂,该方法可在其主要代谢物和/或杂质4-羟基苯甲酸存在的情况下进行。在一根内径75μm、填充5μm C18固定相的毛细管中对分离条件进行了优化,研究了流动相pH值和组成(缓冲液类型和有机溶剂含量)的影响。流动相为5 mM甲酸铵,pH 3.0,含65%乙腈,采用短端进样法(分离毛细管有效长度8 cm),可在不到2.5分钟内实现对混合物中甲酯、乙酯、丙酯、丁酯和苄酯的基线分离,且具有重复性和线性。在最佳实验条件下,该方法对羟基苯甲酸酯类具有较高的分离效率,每米理论塔板数在129312 - 140325之间,分析物定量限(LOQ)在1.25 - 2.50μg/mL范围内。该方法通过直接进样或经过简化的样品预处理,成功应用于制药和化妆品工业样品中对羟基苯甲酸酯类防腐剂的定量分析。