A molecularly imprinted polymer has been synthesized for a selective on-line catechol extraction, followed by its spectrophotometric determination in guarana powder, mate tea and tap water samples. A clean-up column, containing a methacrylic polymer + C 18 solid phase, was also used in order to enhance selectivity. The imprinted polymer was prepared by bulk polymerization using catechol as template and 4-vinylpyridine as the functional monomer. Permanganate solution was used as spectrophotometric reagent, where Mn(VII) was reduced to Mn(II) by catechol in an acid medium, causing color loss, which was monitored at 528 nm. Physical (extraction flow rate, elution flow rate, coil length) and chemical (nature and concentration of the eluent, potassium permanganate concentration) variables were optimized, and the selectivity was appraised using three molecules (4-chloro-2-methylphenol, 2-cresol, 2-methoxyphenol) similar to catechol. These molecules did not present interference in 1:8, 1:10 and 1:10 (catechol/concomitant) proportions, respectively. The analytical calibration curve ranged from 3.0 up to 100 μmol L − 1 ( r > 0.999; seven concentrations levels, n = 3) and the limits of detection (LOD) and quantification (LOQ) were 0.8 and 2.7 μmol L − 1 , respectively. Precision, expressed as RSD, was of 3.0% (20 μmol L − 1 , n = 10), and the analytical frequency was 15 h − 1 . Accuracy was checked by the HPLC technique and the results did not present significant difference at 95% confidence levels according to the t test.
Microchemical Journal – Elsevier
Published: Apr 1, 2007
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