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  • Sensitive headspace gas chromatography-mass spectrometry determination of trihalomethanes in urine.

Sensitive headspace gas chromatography-mass spectrometry determination of trihalomethanes in urine.

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2006-11-10)
J Caro, A Serrano, M Gallego
ABSTRACT

A sensitive and straightforward method for the determination of trihalomethanes (THMs) in urine by using headspace extraction technique has been developed. Chemical and instrumental variables were studied in order to optimize the method for sensitivity: an excess of KCl (4 g per 12 ml of urine), an oven temperature of 85 degrees C and an equilibration time of 30 min were selected. The use of the mass spectrometer in selected ion monitoring mode allows achieving linear ranges between 10 and 5000 ng/l and detection limits from 3 to 10 ng/l, for 12 ml of urine. The stability of the urine sample during storage at 4 and -20 degrees C was also evaluated: THMs remained stable for up to 2 days and 2 months, respectively. Finally, the method was successfully applied to study the THM uptake from swimmers of an indoor swimming pool, as well as non-swimmers. This study revealed that the concentrations of THMs in urine increased approximately three times for chloroform and bromodichloromethane after swimming activity. In addition, THMs in unchanged form were mainly excreted within 2-3h after the end of exposure.

MATERIALS
Product Number
Brand
Product Description

Supelco
Bromoform solution, certified reference material, 5000 μg/mL in methanol
Sigma-Aldrich
Bromodichloromethane, ≥97%
Sigma-Aldrich
Dibromochloromethane, 97%
Sigma-Aldrich
Bromoform, contains 60-120 ppm 2-methyl-2-butene as stabilizer, 99%
Sigma-Aldrich
Bromoform, contains 1-3% ethanol as stabilizer, 96%
Supelco
Bromoform, amylene stabilized, analytical standard