Analysis of PCDD/Fs in environmental samples by using gas chromatography in combination with high resolution mass spectrometry: optimization of sample preparation

ABSTRACTThis study developed a simple, economical and time-saving clean-up procedure based on an in-house packed column system for the determination of the most toxic-relevant 17 PCDD (polychlorinated dibenzo-p-dioxin) and PCDF (polychlorinated dibenzofuran) congeners in environmental samples following accelerated solvent extraction. The extract solution was cleaned up using a manually packed column system consisting of a multi-layer silica gel column and an activated carbon column. After clean-up, dioxins and furans were analysed by using gas chromatography in combination with high-resolution mass spectrometry. Isotopic labelled spiking experiments investigated the recovery of all dioxin and furan congeners. Then, the clean-up procedure for environmental samples was validated by applying the analysis of both clean soil reference material (CRM EDF-5183) and heavily contaminated sediment reference material (CRM EDF-5184) samples, as well as participating in the proficiency test (PT) for sediment samples. The recovery efficiency of isotope-labelled standard compounds in certified reference material (CRM) samples and PT samples ranged from 35% to 101% and between 46.1% and 105%, respectively. The mass concentrations of 17 PCDD/Fs in CRM samples were in the acceptable range. The absolute z-score value for each PCDD/F congener in the PT samples was below 1, confirming the analytical procedure’s high accuracy. The applied clean-up procedure in this study has demonstrated accuracy, repeatability and a significant increase in sample extraction/preparation productivity by reducing the time for sample preparation.KEYWORDS: PCDDsPCDFsclean-up proceduremulti-layer silica gel clean-up columnenvironmental samples Disclosure statementNo potential conflict of interest was reported by the author(s).Supplementary dataSupplemental data for this article can be accessed online at https://doi.org/10.1080/03067319.2023.2260987.Additional informationFundingThis work was supported by component 5: “Improving the quality of dioxin analysis laboratory to international standards”, code [TĐDIOX.05/22-24], under the key science and technology project of VAST: “Research on the risk of dioxin accumulation and derivatives arising from some socio-economic activities to the food production chain”, code: [TĐDIOX.00/22-24]. Nguyen Thi Xuyen was funded by Vingroup JSC and supported by the Master, PhD Scholarship Programme of Vingroup Innovation Foundation (VINIF), Institute of Big Data, code [VINIF.2021.TS.124].