Determination of propranolol and carvedilol in urine samples using a magnetic polyamide composite and LC-MS/MS.
OBJECTIVE
β-blockers are compounds that bind with adrenoreceptors hindering their interaction with adrenalin and noradrenalin. They are clinically relevant and they are also used in some sport as doping agents.


RESULTS
A new method based on the combination of dispersive micro-solid phase extraction and LC-MS/MS has been developed to determine propranolol and carvedilol in urine samples. For this purpose a magnetic-polyamide composite is synthesized and used as sorbent. Working under the optimum conditions, the method provides limits of detection and quantification in the range of 0.1-0.15 μg/l and 0.3-0.5 μg/l, for carvedilol and propranolol, respectively. The precision, expressed as RSD, was better than 9.6% and the relative recoveries varied between 73.7 and 81.3%.


CONCLUSIONS
The methodology is appropriate for the determination of β-blockers in urine samples at the low microgram per liter range for therapeutic purposes.
Department of Analytical Chemistry, Institute of Fine Chemistry & Nanochemistry, Marie Curie Building, Campus of Rabanales, University of Córdoba, 14071 Córdoba, Spain.
Tamara
T
Ballesteros-Esteban
Department of Analytical Chemistry, Institute of Fine Chemistry & Nanochemistry, Marie Curie Building, Campus of Rabanales, University of Córdoba, 14071 Córdoba, Spain.
Emilia M
EM
Reyes-Gallardo
Department of Analytical Chemistry, Institute of Fine Chemistry & Nanochemistry, Marie Curie Building, Campus of Rabanales, University of Córdoba, 14071 Córdoba, Spain.
Rafael
R
Lucena
Department of Analytical Chemistry, Institute of Fine Chemistry & Nanochemistry, Marie Curie Building, Campus of Rabanales, University of Córdoba, 14071 Córdoba, Spain.
Soledad
S
Cárdenas
Department of Analytical Chemistry, Institute of Fine Chemistry & Nanochemistry, Marie Curie Building, Campus of Rabanales, University of Córdoba, 14071 Córdoba, Spain.
Miguel
M
Valcárcel
D000319:Adrenergic beta-Antagonists / Q000652:urine*; D002227:Carbazoles / Q000302:isolation & purification / Q000652:urine*; D000077261:Carvedilol; D002851:Chromatography, High Pressure Liquid; D006801:Humans; D006863:Hydrogen-Ion Concentration; D057230:Limit of Detection; D008280:Magnetics; D008855:Microscopy, Electron, Scanning; D009757:Nylons / Q000737:chemistry; D009994:Osmolar Concentration; D011412:Propanolamines / Q000302:isolation & purification / Q000652:urine*; D011433:Propranolol / Q000302:isolation & purification / Q000652:urine*; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry; D016482:Urinalysis / Q000379:methods*
D000319:Adrenergic beta-Antagonists; D002227:Carbazoles; D009757:Nylons; D011412:Propanolamines; D000077261:Carvedilol; D011433:Propranolol
composite; dispersive micro-solid phase extraction; β-blockers