DETERMINATION OF β-BLOCKERS BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY COUPLED WITH SOLID PHASE MICROEXTRACTION FROM URINE AND PLASMA SAMPLES

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Abstract
The solid phase microextraction (SPME) method was applied to drug monitoring of β-blockers in human urine and plasma. Six β-blockers (alprenolol, atenolol, oxprenolol, pindolol, β-propranolol, and timolol) were extracted from urine and plasma samples by SPME fiber coated with 85-μm polyacrylate for 2 h at 30°C. The β-blockers extracted were separated by Capcell PackTM SG120 (4.6 × 150 mm, 5 μm) with 0.05 M phospholic acid-methanol (55 + 45, v/v) and detected by photometric detection (280 nm) and fluorometric detection (excitation wavelength 220 nm, emission wavelength at 360 nm). The recoveries of β-blockers (500 μg/ml) from urine were 84.3 to 88.4%, and from plasma they were 86.4 to 90.2%. The detection limits were 2 to 25 μg/ml by the photometric detection, 0.4 μg/ml of β-propranolol by fluorescence detection. The relative standard deviations were 10.1 to 15.3% for 500 μg/ml β-blockers in urine, 9.9 to 13.2% for 5 μg/ml of β-blockers in plasma, respectively.

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