Determination of Conditions for Derivatization and Chromatographic Analysis before Simultaneous Analysis of Chloroveratroles and Pentafluorobenzyl Derivatives of Chlorocatechols and Chloroguaiacols in Environmental and Food Samples

Gas chromatography–mass spectrometry and gas chromatography with electron-capture detection have been investigated for analysis of persistent chlorinated aromatic compounds in the aquatic environment. A range of polychlorinated veratroles, guaiacols, and catechols produced during pulp bleaching and during PCB degradation were derivatized with pentafluorobenzyl bromide to improve their chromatographic properties. The reaction was conducted in the presence of triethylamine as neutralization reagent and the derivatized standards obtained were used to estimate the linear range, detection limits, and precision of the method. The conditions used for the derivatization reaction and for chromatographic analysis were optimized. Detector response for the derivatized guaiacols was a linear function of concentration in the range 0.5–100 ng mL; for chloroguaiacols and underivatized chloroveratroles the range was 0.5 to 80 ng mL. Detection limits ranged from 0.18 ng mL for tetrachlorocatechol (TeCC) to 2.72 ng mL for 4-chloroguaiacol (4-CG). GC–MS was used for final confirmation of the identity of the compounds analyzed.