Automated determination of total captopril in urine by liquid chromatography with post-column derivatization coupled to on-line solid phase extraction in a sequential injection manifold

作者：Karakosta Theano D; Tzanavaras Paraskevas D; Themelis Demetrius G^*

来源：Talanta, 2012, 88: 561-566.

DOI：10.1016/j.talanta.2011.11.034

• Captopril
• Post-column derivatization
• Human urine
• Ethyl propiolate
• Automated solid phase extraction

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 mu g L-1 and 35 mu g 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.

• 出版日期2012-1-15