Journal
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 407, Issue 7, Pages 2013-2022Publisher
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-015-8464-1
Keywords
Magnetic-stirring-assisted dispersive liquid-liquid microextraction; Multisyringe chromatography; Phenolic compounds; Environmental samples; Automation
Funding
- Spanish Ministry of Economy and Competitiveness (MINECO) [CTQ2013-47461-R]
- FEDER
- Conselleria d'Economia, Hisenda, I Innovacio of the Government of the Balearic Islands [43/2011]
- European Funds [PTQ-2012-05755]
- Torres Quevedo Program of MINECO
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An automatic phenolic compounds analyzer is presented. The system performs online magnetic-stirring-assisted dispersive liquid-liquid microextraction before multisyringe chromatography (MSC) using a monolithic Chromolith Flash RP-18e column. The extraction behavior of the following phenolic pollutants: phenol, 2-nitrophenol, 4-nitrophenol, 2-chlorophenol, 2,4-diclorophenol, and 2,4,6-trichlorophenol, has been studied. A critical comparison of extractants (tributyl phosphate, acetonitrile, hexane, and 1-chlorobutane) and disperser solvents (acetone, acetonitrile, ethanol, methanol, 1-propanol, and 2-propanol) was made. Tributyl phosphate and acetonitrile were chosen as the extractant and the disperser solvent, respectively, since these showed the best performance. Phenols were online back-extracted into NaOH and neutralized before multi-isocratic chromatographic separation. The proposed analyzer can be applied for wide linear working ranges, i.e., between 40 and 20,000 mu g L-1. The precision of the developed system has been proved, with maximum values for the intraday and interday precision of 4.4 % and 5.2 %, respectively, expressed as relative standard deviation, and high preconcentration factors (9.3-10.5) for most of the compounds studied. The method developed was successfully applied to natural water samples.
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