Ion-pair single-drop microextraction versus phase-transfer catalytic extraction for the gas chromatographic determination of phenols as tosylated derivatives (Journal article)

Fiamegos, Y. C./ Kefala, A. P./ Stalikas, C. D.

The environmental fate of phenols represents a diachronic scientific consideration mainly due to their high toxicity and diverse physicochemical properties rendering them difficult to be analyzed as unity. Ion-pair-assisted extraction and microextraction techniques in association with a dedicated derivatization reaction are possible to lead to enhanced selectivity and sensitivity in gas chromatography. Phase-transfer catalytic liquid-liquid extraction-derivatization and ion-pair-assisted single-drop microextraction with in-drop derivatization are successfully employed for the analysis of 15 phenolic compounds. The analytes that react at room temperature with p-toluenesulfonyl chloride into the bulk of the organic phase are subsequently determined by GC-MS in selective-ion monitoring mode. Aiming at maximizing the derivatization yields obtained from the 15 analytes in a reasonable time period, the optimum experimental parameters were established along with the figures of merit of the methods. The limits of detection ranged from 0.48 to 1.5 ng/ml and from 0.20 to 0.28 ng/ml respectively, while the limits of quantitation ranged from 1.4 to 4.5 ng/ml and from 0.59 to 0.84 ng/ml for the two methods with the techniques under study. The overall procedure presented satisfactory analytical features with the liquid-liquid extraction protocol being easier to carry out while the single-drop one, presented higher sensitivity and significant reduction of the organic solvent employed. By comparison with other methods for the analysis of phenols, the proposed methods exhibit adequately low detection limits, good precision, short derivatization time and low solvent, sample and reagent consumption. (C) 2008 Elsevier B.V. All rights reserved.
Institution and School/Department of submitter: Πανεπιστήμιο Ιωαννίνων. Σχολή Θετικών Επιστημών. Τμήμα Χημείας
Keywords: phenols,p-toluenesulfonyl chloride,phase-transfer catalysis,ion-pair,single-drop microextraction,preconcentration,derivatization,mass-spectrometric detection,water samples,liquid-chromatography,spectrophotometric determination,endocrine disruption,trace concentrations,selective detection,derivatization,ionization,chlorophenols
ISSN: 0021-9673
Link: <Go to ISI>://000255848600007
Publisher: Elsevier
Appears in Collections:Άρθρα σε επιστημονικά περιοδικά ( Ανοικτά)

Files in This Item:
File Description SizeFormat 
Fiamegos-2008-Ion-pair single-drop.pdf413.62 kBAdobe PDFView/Open    Request a copy

 Please use this identifier to cite or link to this item:
  This item is a favorite for 0 people.

Items in DSpace are protected by copyright, with all rights reserved, unless otherwise indicated.