High performance solid-phase analytical derivatization of phenols for gas chromatography-mass spectrometry.
The solid-phase analytical derivatization of phenols with pentafluoropyridine is performed. Fourteen phenols including chlorophenols and alkylphenols, could be efficiently adsorbed on a strong anion-exchange solid phase, Oasis MAX. The phenols adsorbed on Oasis MAX as phenolate ions were desorbed after derivatization with pentafluoropyridine. After optimization of the adsorption and derivatization, we established a procedure for the determination of the phenols in water samples by means of GC-MS. Under the optimized conditions, calibration curves were linear in the range of 10-1000 ng/l for the alkylphenols (100-10000 ng/l for nonylphenol) and 50-1000 ng/l for the others. By processing 100 ml samples, the method detection limits (MDLs) were in the range of 0.45-2.3 ng/l for the alkylphenols (8.5 ng/l for nonylphenol) and 2.4-16 ng/l for the others. Compared with the biphasic reaction system, the signal-to-noise ratios obtained by the solid-phase analytical derivatization were significantly higher. This is ascribed to the fact that coexisting neutral and acidic compounds are efficiently removed from the sample solution by this solid-phase analytical derivatization system.
Research Center for Environmental Preservation, Osaka University, Yamada-oka 2-4, Suita, Osaka 565-0871, Japan.
Miki
M
Kojima
Shinji
S
Tsunoi
Minoru
M
Tanaka
D000042:Absorption; D002138:Calibration; D005618:Fresh Water / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry; D007202:Indicators and Reagents; D007700:Kinetics; D010636:Phenols / Q000032:analysis*; D011725:Pyridines / Q000737:chemistry; D011786:Quality Control; D015203:Reproducibility of Results; D012972:Sodium Hydroxide / Q000737:chemistry; D014874:Water Pollutants, Chemical / Q000032:analysis; D005466:Fluorocarbons
D007202:Indicators and Reagents; D010636:Phenols; D011725:Pyridines; D012972:Sodium Hydroxide; D014874:Water Pollutants, Chemical; C486857:pentafluoropyridine; D005466:Fluorocarbons