Determination of selected β-receptor antagonists in biological samples by solid-phase extraction with cholesterolic phase and LC/MS

Abstract

A new method is presented for the determination of five selected beta-receptor antagonists by HPLC, which emphasizes sample preparation via retention on a new type of silica gel sorbent used for solid-phase extraction (SPE). Sorbents of this type were obtained by the chemical modification of silica gels of various porosities by cholesterol ligands. The cholesterol-based packing material was investigated by spectroscopic methods and elemental analysis. The recoveries obtained with the extraction procedure were optimum over a relatively broad sample pH range (3.08-7.50). Analytical factors such as the sample loading, the washing step and elution conditions, the concentration of beta-receptor antagonists to be extracted, and the type of sorbent were found to play significant roles in the sample preparation procedure and would therefore need to be controlled to achieve optimum recoveries of the analytes. Under optimum conditions, the recoveries of nadolol, acebutolol, esmolol, oxprenolol and propranolol from spiked buffers, blood and urine were reproducible and dependent on the polarity or hydrophilicity of the compounds. The above analytes were determined by reverse-phase high-performance liquid chromatography (HPLC) with UV and ESI-ion trap mass spectrometry (MS) detection. The described method was found to be suitable for the routine measurement of compounds that are both polar and basic, and can be applied for the analysis of biological samples such as urine and blood in clinical, toxicological or forensic laboratories. The recovery measurements were performed on spiked human urine and serum, and on real samples of mouse blood serum.

New alkyl-phosphate bonded stationary phases for liquid chromatographic separation of biologically active compounds

“…The results were much worse than for the Amino-P-C10 stationary phase. However, the beta-blockers can be separated on Amino-Cholesterol stationary phases by use of gradient elution with a buffered mobile phase [37]. Use of Amino-P-C10 enables separation without addition of buffer to the mobile phase.…”

UHPLC method for the simultaneous determination of β-blockers, isoflavones and their metabolites in human urine

“…Separation has been achieved with either conventional LC [7][8][9][10][11][12][13][14][15][16] or ultrahigh performance liquid chromatography (UPLC) [17]. Moreover, several methods utilizing low resolution MS have been published [7][8][9][10][11][12][13][14][15][16].…”

“…Separation has been achieved with either conventional LC [7][8][9][10][11][12][13][14][15][16] or ultrahigh performance liquid chromatography (UPLC) [17]. Moreover, several methods utilizing low resolution MS have been published [7][8][9][10][11][12][13][14][15][16]. A UV-vis detector, particularly those in a diode-array configuration [18][19][20][21][22][23][24], fluorescence detector [24][25][26][27][28][29][30] and electrochemical detector [31] are the most widely utilised detectors with HPLC.…”

Determination of landiolol, an ultra-short-acting β1-receptor antagonist, in human plasma by liquid chromatography–tandem mass spectrometry

“…Numerous anesthetic drugs and techniques have been developed to minimize and treat acute hemodynamic responses during surgery [1,2] with short-acting adrenergic ␤ 1 -receptor antagonists being one of the most effective. Administration of this type of drug allows an adequate depth of anesthesia to be achieved with less anesthetic and less demand for postoperative analgesia [3,4].…”