Simultaneous determination of short-chain chlorinated paraffins and other classes of persistent organic pollutants in sediment by gas chromatography‒tandem mass spectrometry after ultrasonic solvent extraction combined with stir bar sorptive extraction
The study presents a fast and high throughput method for determination of short-chain chlorinated paraffins (SCCPs) together with other halogenated persistent organic pollutants (POPs) in sediment. The analytes (SCCPs, 11 polychlorinated biphenyls, 6 polybrominated diphenyl ethers, 11 organochlorine compounds) were determined in a single gas chromatography‒triple quadrupole tandem mass spectrometry (GC‒QqQ-MS/MS) run after miniaturized sample preparation combining ultrasonic solvent extraction (USE) and stir bar sorptive extraction (SBSE). The method was validated in terms of selectivity, matrix effect, matrix-matched recovery, linearity and range, detection and quantification limits (LOD and LOQ) and accuracy (including analysis of certified reference materials). The QqQ-MS/MS detector allowed the determination of all target analytes without interferences. The LODs and LOQs for SCCPs were 6.5 and 22 ng g‒1 dw (dry weight), while for other analytes were in the ranges 0.029‒0.073 ng g‒1 and 0.097‒0.24 ng g‒1, respectively. The recoveries for all the analytes were in the range 84‒101% with relative standard deviations in the range 5.5‒19%. In terms of environmental impact, the method was classified as “an excellent green analysis method”. Finally, the method was compared with other published methods and its applicability was confirmed by the analysis of sediment samples collected in 23 Slovak water reservoirs during a survey conducted in 2019.
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Keywords: Short-chain chlorinated paraffins; Persistent organic pollutants; Sediment extraction; Stir bar sorptive extraction; Thermal desorption; Gas chromatography–tandem mass spectrometry