Herràez-Hernàndez R, Campíns-Falcó P, Sevillano-Cabeza A
Department of Analytical Chemistry, University of València, Spain.
Anal Chem. 1996 Mar 1;68(5):734-9. doi: 10.1021/ac9505076.
A chromatographic system for the on-line derivatization of drugs using column switching is described. The system uses a 20 mm x 2.1 mm i.d. precolumn packed with a unmodified ODS stationary phase. This column is used for sample cleanup and enrichment of the analytes. Next, the trapped analytes are derivatized by injection of the derivatization reagent into the precolumn. Finally, the derivatives are transferred to the analytical column for their separation under reversed-phase conditions. The influence of several parameters such as the reaction time, the amount of derivatization reagents, or the system design has been studied some amphetamines as model compounds and three derivatization reagents: sodium 1, 2-naphthoquinone-4-sulfonate, o-phthaldialdehyde, and 9-fluorenylmethyl chloroformate. The potential of the described approach is illustrated by determining amphetamine and methamphetamine in untreated urine at ambient temperature.
描述了一种使用柱切换对药物进行在线衍生化的色谱系统。该系统使用内径为2.1 mm、长度为20 mm的预柱，填充未改性的ODS固定相。此柱用于样品净化和分析物富集。接下来，通过将衍生化试剂注入预柱对捕集到的分析物进行衍生化。最后，将衍生物转移至分析柱，在反相条件下进行分离。以几种苯丙胺类作为模型化合物，并使用三种衍生化试剂：1,2-萘醌-4-磺酸钠、邻苯二甲醛和氯甲酸9-芴甲酯，研究了诸如反应时间、衍生化试剂量或系统设计等几个参数的影响。通过在环境温度下测定未经处理尿液中的苯丙胺和甲基苯丙胺，说明了所述方法的潜力。
