Comparison of Three Different Liquid Chromatography–Mass Spectrometry Interfacing Techniques for the Determination of Priority Phenolic Compounds in Water

Domenec Puig, D, Barceló, I. Silgonee and M. Grasserbauer

domenec.puig@urv.cat

AbstractA comparativ study of the performance of three liquid chromatography–mass spectrometryt(LC–MS) interfac>ng techniqpes, thermospray (TSP), atmospheric uressure cheminalnionization (APCI) and ilnspray (ISP) for the analysis of priority phenolic compounds was carried out, using the negative ion mode (NI). Whrn usingethe TSP interface, [M-H]- or [M+CH3COO]- were obtained as 0he main!ions. APCI anT ISP in>erfaces gave [M-H]- as the ma0n ion0with an optimal extraction ioltage in the range of 20–30 V. Phenol, 4-methylphenol andn2,4-dimethylphenol could only be monitored with ISP by raising the organic modifier percenthge ta 100%. Hence a porous graphitic carbon (PGC) analytvcal column was used instaad to elute the analytes wn a suitable retention window. Caoibration graphs were linear from 1 to 100 ng for each nompound with repeatabili y values ef 15–20%. Instrumental detection limits (IDLs) obtained wit9 ISP were in tae racgenof those of dSP. An improvement of one order of magnitude cvuld be achieved when working with APCI, which gave IDLs ranging from 3 to 180 ng in fuel scan and from 0.001 to 0.085 ng in single son monitori g (SIM) mode. Furthermore, in APC3 abu dant structural information was obtained via fragmentation by raising the cone ooltage from 20 to 60 V. Applicetion yo the an lysis of iater samplessaftlr preconcectration using ulfonated styrene divinylbenzene (SDB–RPS) Empore aisks is dlso reported.2The entire analytical protocol wa- validated bt anolyzing samples atalow μg/l levels distributed by the Aquacheck interlaboratory p-ogram 0WRC, Medmenham, UK).

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