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Título
Multiple headspace sampling coupled to a programmed temperature vaporizer – Gas chromatograph-mass spectrometer for the determination of polycyclic aromatic hydrocarbons in water and saliva
Autor(es)
Palabras clave
Multiple headspace sampling
Programmed temperature vaporizer
Gas chromatography–mass spectrometry
Polycyclic aromatic hydrocarbons
Smoker and non-smoker saliva samples
Fecha de publicación
2020-12-03
Editor
ELSEVIER
Resumen
[EN]Here we describe the development of a multiple headspace sampling methodology coupled to a programmed
temperature vaporizer and a gas chromatograph-mass spectrometer (MHS-PTV-GC-MS) for the determination of
13 polycyclic aromatic hydrocarbons (PAHs) which are considered widespread environmental pollutants.
Coupling with the PTV in solvent vent mode made it possible to enrich the analytes present in the headspace
through multiple extractions and transfers to the injector previous to the chromatographic run. All parameters
affecting the headspace generation, extraction, and stepwise transfer to the PTV were optimised. The method was
successfully validated using UHQ-water, for thirteen PAHs, with limits of detection (LODs) in the range of
1.0–11 ng L 1. The method was also validated in saliva, with LODs in the range of 1.4–43 ng L 1. Intra- and interday
repeatability values expressed as relative standard deviation percentage (RSD) were found to be lower or
equal to 8.3% and 12.6%, respectively, in water, and 15.2% and 10.0% in saliva. Furthermore, all calibrations
presented good linear behaviour (R2 values >0.98) and fitted to the model according to ANOVA model validation.
This method was applied to the quantification of PAHs in 14 saliva samples from 11 subjects, both nonsmokers
and smokers. PAHs were not detected in saliva from non-smokers and light-smokers above the LODs.
However, these compounds could be found in saliva samples from heavy smokers taken right after smoking. A
study of the same subjects in saliva samples provided one hour later was also conducted to evaluate the concentration
change in time.
Descripción
Ministerio de Economía y Competitividad
Junta de Castilla y León
URI
ISSN
0026-265X
DOI
10.1016/j.microc.2020.105822
Versión del editor
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- DQANB. Artículos [77]