On-line molecularly imprinted solid phase extraction for the selective spectrophotometric determination of catechol

On-line molecularly imprinted solid phase extraction for the selective spectrophotometric... 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. http://www.deepdyve.com/assets/images/DeepDyve-Logo-lg.png Microchemical Journal Elsevier

On-line molecularly imprinted solid phase extraction for the selective spectrophotometric determination of catechol

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Publisher
Elsevier
Copyright
Copyright © 2006 Elsevier B.V.
ISSN
0026-265X
eISSN
1095-9149
D.O.I.
10.1016/j.microc.2006.07.004
Publisher site
See Article on Publisher Site

Abstract

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.

Journal

Microchemical JournalElsevier

Published: Apr 1, 2007

References

  • Anal. Chim. Acta
    Lai, J.P.; Niessner, R.; Knopp, D.
  • Anal. Chem.
    Wu, W.; Ashley, D.L.; Watson, C.H.
  • Analyst
    Analytical Methods Committee
  • Anal. Chim. Acta
    Dantoni, P.; Serrano, S.H.P.; Brett, A.M.O.; Gutz, I.G.R.

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