title: Direct doping analysis of beta-blocker drugs from urinary samples by on-line molecularly imprinted solid-phase extraction coupled to liquid chromatography/mass spectrometry.
abstract: The use of beta-blockers to enhance performance in some sports is forbidden. Based on this regulation, there is a demand for dynamic analytical procedures for analyzing these compounds quickly and without manual sample preparation. Therefore, the use of a molecularly imprinted polymer (MIP) in a multidimensional liquid chromatographic system coupled to a mass spectrometer provides a good alternative for improving the selectivity and practicality of the beta-blocker analyses, as described in this paper. A water-compatible MIP for oxprenolol was synthesized by the precipitation method, using methacrylic acid as a functional monomer and 2-hydroxyethyl methacrylate and glycerol dimethacrylate as hydrophilic monomers. A column filled with MIP was coupled to an LC-MS/MS instrument under the multidimensional configuration, with 10.0 mmol L(-1) ammonium formate buffer (pH 5.0) as the loading and reconditioning mobile phase and a 0.01% formic acid aqueous solution-methanol (30 : 70 v : v) as the elution mobile phase. The system was used for on-line extraction and quantization of oxprenolol (from 1.0 to 75.0 μg L(-1)), atenolol, propranolol, nadolol, pindolol, labetalol and metoprolol (all from 3.0 to 50 μg L(-1)) simultaneously, from urine samples. The correlation coefficient was higher than 0.99 for all the analytes. Suitable precision and accuracy were obtained.
authors: Toxicants and Drugs Analysis Laboratory - LATF, Faculty of Pharmaceutical Sciences, Federal University of Alfenas - Unifal-MG, 700 Gabriel Monteiro da Silva Street, 37130-000, Alfenas, MG, Brazil. eduardocfig@yahoo.com.br.
authors: Mariane Gonçalves
authors: MG
authors: Santos
authors: Isabela Maria Campos
authors: IM
authors: Tavares
authors: Vanessa Bergamin
authors: VB
authors: Boralli
authors: Eduardo Costa
authors: EC
authors: Figueiredo
mesh_terms: D000319:Adrenergic beta-Antagonists / Q000032:analysis* / Q000302:isolation & purification*; D002853:Chromatography, Liquid / Q000379:methods*; D004300:Doping in Sports; D005990:Glycerol / Q000737:chemistry; D006801:Humans; D008689:Methacrylates / Q000737:chemistry; D054802:Molecular Imprinting / Q000379:methods*; D011108:Polymers / Q000138:chemical synthesis / Q000737:chemistry; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D016482:Urinalysis / Q000379:methods*
chemical_list: D000319:Adrenergic beta-Antagonists; D008689:Methacrylates; D011108:Polymers; C008384:methacrylic acid; C005044:hydroxyethyl methacrylate; D005990:Glycerol