Ion-pair solid-phase extractive derivatization of 4-alkylphenols with pentafluoropyridine for gas chromatography-mass spectrometry.
The ion-pair solid-phase extraction (SPE) of 4-alkylphenols followed by derivatization with pentafluoropyridine is demonstrated. Under alkaline conditions, the 4-alkylphenols could be efficiently adsorbed on a C18 SPE cartridge conditioned with an ion-pair reagent, tetra-n-hexylammonium bromide. The ion pairs, ammonium phenolates, formed on the C18 solid phase, were eluted with a solvent containing the derivatizing reagent, pentafluoropyridine, and completely derivatized during the elution. After optimization of the adsorption and derivatization, we established a method for the determination of the 4-alkylphenols in water samples. The method showed good linearity between 20 and 1000 ng (200-10,000 ng for nonylphenol). By processing 20-ml samples, the method detection limits (MDL) were in the range of 5.2-8.9 ng/l for the 4-alkylphenols (76 ng/l for nonylphenol). To evaluate its applicability to a real aqueous matrix, several river water samples were analyzed.
Kojima
Miki
M
Research Center for Environmental Preservation, Osaka University, 2-4 Yamada-oka, Suita, Osaka 565-0871, Japan.
Matsui
Norie
N
Tsunoi
Shinji
S
Tanaka
Minoru
M
D008401:Gas Chromatography-Mass Spectrometry; D010636:Phenols / Q000737:chemistry* / Q000302:isolation & purification*; D011725:Pyridines / Q000737:chemistry*; D015203:Reproducibility of Results; D014874:Water Pollutants, Chemical / Q000032:analysis / Q000302:isolation & purification; D005466:Fluorocarbons
D010636:Phenols; D011725:Pyridines; D014874:Water Pollutants, Chemical; C486857:pentafluoropyridine; D005466:Fluorocarbons