Simultaneous determination of the full chlorophenol spectrum in human urine using gas chromatography with tandem mass spectrometry

•The procedure enables for the first time the simultaneous trace analysis of the full spectrum of 19 chlorophenols in urine.•Separation using an intermediate polarity arylene polysiloxane column combined with MS/MS permits resolution of all isomers.•The high sensitivity of the procedure with LOD of 0.01-0.03 μg/L suggests its application in population studies.

The determination of chlorophenols in urine is an established approach for the assessment of human exposure to these ubiquitous environmental pollutants. However, an analytical procedure which enables the separate determination of all components of this substance group was still lacking. For this task we developed a method using enzymatic hydrolysis, solid phase extraction, derivatisation with bis(trimethylsilyl)trifluoroacetamide and gas chromatography-tandem-mass spectrometry with isotope dilution. The chromatographic conditions provided baseline separation of all 19 chlorophenol derivatives. Precision within series did not exceed 15% although for urinary concentrations of 1 μg L−1. The recovery was found to be well for most of the parameters. Limits of quantifications ranged between 0.04 and 0.10 μg L−1. The present method is the first procedure which enables the simultaneous trace analysis of the full spectrum of chlorophenols in human urine. Thus, it may be a suitable benchmark procedure for the human biomonitoring of the exposure to these compounds in population studies.

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