Determination of alkylphenols in water samples using liquid chromatography–tandem mass spectrometry after pre-column derivatization with dansyl chloride
2015
Pernica, Marek | Poloucká, Petra | Seifertová, Marta | Šimek, Zdeněk
The present study describes an effect of reaction condition of pre-column derivatization of alkylphenols (APs): bisphenol A (BPA), 4-tert-octylphenol (4-t-OP), 4-octylphenol (4-OP), 4-n-nonylphenol (4-n-NP), and isomers of 4-nonylphenol (iso-NP) with 5-(dimethylamino) naphthalene-1-sulfonyl chloride (dansyl chloride, DNSC) on their LC–ESI–MS/MS determination in water samples. Chemical derivatization improves the sensitivity and selectivity of LC–MS/MS analysis. In principle, alkylphenols can be analyzed by LC–MS/MS without derivatization. However, pre-column derivatization of APs increases the sensitivity up to 1000 times in comparison with the analysis of underivatized alkylphenols. Reaction conditions affecting formation of the DNSC-derivatives, such as various solvent, reaction temperature, reaction time, DNSC concentration and pH values were tested. The most suitable conditions, in terms of achieving a high sensitivity, resulting from this study are: acetonitrile as reaction solvent, 60min as reaction time, 60°C as reaction temperature, pH values 10.5, 0.5mgmL⁻¹ as DNSC concentration. Calibration curves are linear at least in the range of 1–1000ngmL⁻¹, limits of detection (LOD) and limits of quantification (LOQ) ranging from 0.02 to 0.25pg/injection and from 0.08 to 0.83pg/injection, respectively. The improved procedure was successfully applied for the analysis of APs and BPA in real water samples. The median concentration of BPA and iso-NP obtained in bottled waters was 4.7ngL⁻¹ and 33.5ngL⁻¹, respectively. The median concentration of 4-t-OP was 1.3ngL⁻¹.
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