کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
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5136194 | 1494002 | 2017 | 12 صفحه PDF | دانلود رایگان |
- A rational synthesis of molecularly imprinted polymer showed great potential and high recovery.
- A simple PT-MIP-SPE was developed to extract carvedilol enantiomers from human urine samples.
- Enantioseparation of carvedilol was improved using an immobilized polysaccharide-based chiral stationary phase.
- The method has been applied in a preliminary study of urinary excretion after administration via oral of carvedilol racemate.
In this work, an efficient pipette tip based on molecularly imprinted polymers solid-phase extraction (PT-MIP-SPE) method was developed for carvedilol (CAR) analysis. This compound is available in clinical practice as a racemic mixture, in which (â)-(S)-CAR is a β- and α1-adrenergic antagonist, while (+)-(R)-CAR only acts as an α1-adrenergic antagonist. Enantioseparation of CAR presented satisfactory retention times (5.85 and 14.84 min), acceptable theoretical plates (N = 2048 and 2018) and good resolution (Rs = 9.27). The separation was performed using a Chiralpak® IA column (100 mm Ã 4.6 mm, 3 μm), a mixture of methanol:ethanol:water (64:15:21, v/v/v) plus 0.3% diethylamine as mobile phase, temperature of 35 °C and flow rate of 1.5 mL minâ1. After density functional theory calculations based on prepolymerization complexes, the best protocol for the MIP synthesis was chosen. Then, some parameters that affect the PT-MIP-SPE technique were investigated. After optimization, the best conditions were 300 μL of water as washing solvent, 500 μL of acetonitrile:acetic acid (7:3, v/v) as eluting solvent, 20 mg of MIP, 500 μL of urine sample (pH 12.5) and no addition of NaCl. Recoveries ± relative standard deviation (RSD%) for (+)-(R)-CAR and (â)-(S)-CAR were 101.9 ± 4.8% and 104.6 ± 2.1%, respectively. The method was linear over the concentration range from 20 to 1280 ng mLâ1 for each enantiomer, with correlation coefficients larger than 0.99 for both enantiomers. The method was applied successfully in a preliminary study of urinary excretion after administration of CAR racemate to a healthy volunteer.
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Journal: Journal of Chromatography B - Volumes 1061â1062, 1 September 2017, Pages 399-410