Laboratory of Analytical Chemistry, Department of Chemistry, Aristotelian University of Thessaloniki, GR-54124 Thessaloniki, Greece.
Talanta. 2012 Jan 15;88:561-6. doi: 10.1016/j.talanta.2011.11.034. Epub 2011 Nov 18.
The present study reports a new liquid chromatographic (HPLC) method for the determination of the anti-hypertension drug captopril (CAP) in human urine. After its separation from the sample matrix in a reversed phase HPLC column, CAP reacts with the thiol-selective reagent ethyl-propiolate (EP) in a post-column configuration and the formed thioacrylate derivative is detected at 285 nm. Automated 4-fold preconcentration of the analyte prior to analysis was achieved by an on-line solid phase extraction (SPE) step using a sequential injection (SI) manifold. The Oasis HLB SPE cartridges offered quantitative recoveries and effective sample cleaning by applying a simple SPE protocol. The limits of detection and quantitation were 10 μg L(-1) and 35 μg L(-1) respectively. The percent recoveries for the analysis of human urine samples ranged between 90 and 96% and 95 and 104% using aqueous and matrix matched calibration curves respectively.
本研究报告了一种新的液相色谱（HPLC）法，用于测定人尿中的抗高血压药物卡托普利（CAP）。在反相 HPLC 柱中从样品基质中分离出来后，CAP 在柱后与硫醇选择性试剂乙基丙烯酸盐（EP）反应，形成的硫代丙烯酸盐衍生物在 285nm 处检测到。通过在线固相萃取（SPE）步骤，采用顺序注射（SI）流路，在分析前对分析物进行了 4 倍自动预浓缩。Oasis HLB SPE 小柱采用简单的 SPE 方案，提供了定量的回收率和有效的样品净化。检测限和定量限分别为 10μg/L 和 35μg/L。使用水相和基质匹配校准曲线，人尿样分析的回收率在 90%至 96%和 95%至 104%之间。
