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Efficient Molecularly Imprinted Polymer as a Pipette-Tip Solid-Phase Sorbent for Determination of Carvedilol Enantiomers in Human Urine

Efficient Molecularly Imprinted Polymer as a Pipette-Tip Solid-Phase Sorbent for Determination of Carvedilol Enantiomers in Human Urine

Anny Talita Maria da Silva, Hanna Leijoto de Oliveira, Camilla Fonseca Silva, Matheus Cecílio Fonseca, Thales Fernando Dias Pereira, Clebio Soares Nascimento Jr, Eduardo Costa de Figueiredo, Keyller Bastos Borges

J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Sep 1;1061-1062:399-410.

PMID: 28803116

Abstract:

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 (-)-(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 14.84min), acceptable theoretical plates (N=2048 and 2018) and good resolution (Rs=9.27). The separation was performed using a Chiralpak® IA column (100mm×4.6mm, 3μm), 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 1.5mLmin-1. 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 300μL of water as washing solvent, 500μL of acetonitrile:acetic acid (7:3, v/v) as eluting solvent, 20mg of MIP, 500μL of urine sample (pH 12.5) and no addition of NaCl. Recoveries±relative standard deviation (RSD%) for (+)-(R)-CAR and (-)-(S)-CAR were 101.9±4.8% and 104.6±2.1%, respectively. The method was linear over the concentration range from 20 to 1280ngmL-1 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.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
IAR42141	HPLC PT			Price

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