Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1248, Issue -, Pages 55-59Publisher
ELSEVIER
DOI: 10.1016/j.chroma.2012.05.099
Keywords
Ion-pair in-tube solid-phase microextraction; Reversed-phase TiO2 capillary column; Ion-pair capillary chromatography; Lauralkonium chloride; Surfactants
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A quick, miniaturized and on-line method has been developed for the determination in water of the predominant homologue of benzalkonium chloride, dodecyl dimethyl benzyl ammonium chloride or lauralkonium chloride (C-12-BAK). The method is based on the formation of an ion-pair in both in-tube solid-phase microextraction (IT-SPME) and capillary liquid chromatography. The IT-SPME optimization required the study of the length and nature of the stationary phase of capillary and the processed sample volume. Because to the surfactant character of the analyte both, the extracting and replacing solvents, have played a decisive role in the IT-SPME optimized procedure. Conditioning the capillary with the mobile phase which contains the counter ion (acetate), using an organic additive (tetrabutylammonium chloride) added to the sample and a mixture water/methanol as replacing solvent (processed just before the valve is switched to the inject position), allowed to obtain good precision of the retention time and a narrow peak for C-12-BAK. A reversed-phase capillary based TiO2 column and a mobile phase containing ammonium acetate at pH 5.0 for controlling the interactions of cationic surfactant with titania surface were proposed. The optimized procedure provided adequate linearity, accuracy and precision at the concentrations interval of 1.5-300 mu g L-1. The limit of detection (LOD) was 0.5 mu g L-1 using diode array detection (DAD). The applicability of proposed IT-SPME-capillary LC method has been assessed in several water samples. (c) 2012 Elsevier B.V. All rights reserved.
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