| Title | Simultaneous determination of Chlorinated Priority Organic Pollutants (e.g. PCB, PBDE, PCDD, PCDF) in soil and sediments by Gas Chromatography-Tandem Mass Spectrometry |
| Abstract | Epidemiological studies show that exposure to specific persistent organic pollutants (POPs) such as polychlorinated dibenzo-p-dioxins (PCDD), dibenzofurans (PCDF), polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) is strongly associated with negative interferences on endocrine systems and on alterations of reproductive physiology. Therefore, the determination of these compounds in the environment is of great importance from the ecotoxicological point of view. Accurate determination of PCDD/F, PBDE and PCB in complex matrices is a challenge because of their low expected concentrations in the range of ppb to sub-ppb. For the complexity of environmental matrices, analytical determinations often require long time periods of analysis and several stages of extraction/preconcentration, purification, etc in order to eliminate interferences. These procedures do not fit in extensive environmental monitoring programs, where it is necessary to analyze a large number of samples at a time not excessively long. In this paper, the official EPA methods (1,2) for chlorinated pollutant analysis has been evaluated and modified to provide a faster and more reliable alternative analytical method for simultaneous determination of interest compounds in soil and sediments with a single extraction.
Accelerated solvent extraction (ASE) has been used for simultaneous extraction of organic compounds. The most favorable extraction conditions proved to be n-hexane as the extraction solvent, temperature of 120 °C, pressure of 1500 psi and three static cycles in each case. Purification of the extract was accomplished by automated Power-PrepTM/Sample Clean-up system. The analyses were then performed by using gas chromatography coupled to triple quadrupole mass spectrometry. Utilizing triple quadruple mass spectrometry under positive EI with multiple reaction monitoring (MRM) mode, greatly enhances the sensitivity and selectivity of detection, compared to selective ion monitoring (SIM) mode. The GC-QqQ(MS/MS) sensitivity, lower than that of GC-HRMS, is good enough (LODs in the down to low pg levels) to detect the normal concentrations of these compounds in environmental samples. The obtained analytical results demonstrate excellent recoveries for the various congeners, comparable to those of official methods and detection limits useful for the analysis of real matrices. The determination of these compounds in soils and sediments and the evaluation of the distribution of various congeners (fingerprint method) has allowed to obtain information on the origin of the contamination. |
| Source | XXVI Congresso Nazionale della Società Chimica Italiana, Paestum (SA), 10-14/09/2017 |
| Keywords | PCBPCVDD/FPBDE |
| Year | 2017 |
| Type | Contributo in atti di convegno |
| Authors | Giuseppe Bagnuolob, Francesco Cardellicchioa, Ruggiero Ciannarellab, Vito Lo Caputob, Giuseppe Mascolob, Francesco Palmisanoa |
| Text | 398041 2017 PCB PCVDD/F PBDE Simultaneous determination of Chlorinated Priority Organic Pollutants e.g. PCB, PBDE, PCDD, PCDF in soil and sediments by Gas Chromatography Tandem Mass Spectrometry Giuseppe Bagnuolob, Francesco Cardellicchioa, Ruggiero Ciannarellab, Vito Lo Caputob, Giuseppe Mascolob, Francesco Palmisanoa a Department of Chemistry, University of Bari, Via Orabona 4, 70126 Bari, b CNR IRSA, Via F. De Blasio 5, 70132 Bari; Epidemiological studies show that exposure to specific persistent organic pollutants POPs such as polychlorinated dibenzo p dioxins PCDD , dibenzofurans PCDF , polybrominated diphenyl ethers PBDEs and polychlorinated biphenyls PCBs is strongly associated with negative interferences on endocrine systems and on alterations of reproductive physiology. Therefore, the determination of these compounds in the environment is of great importance from the ecotoxicological point of view. Accurate determination of PCDD/F, PBDE and PCB in complex matrices is a challenge because of their low expected concentrations in the range of ppb to sub ppb. For the complexity of environmental matrices, analytical determinations often require long time periods of analysis and several stages of extraction/preconcentration, purification, etc in order to eliminate interferences. These procedures do not fit in extensive environmental monitoring programs, where it is necessary to analyze a large number of samples at a time not excessively long. In this paper, the official EPA methods 1,2 for chlorinated pollutant analysis has been evaluated and modified to provide a faster and more reliable alternative analytical method for simultaneous determination of interest compounds in soil and sediments with a single extraction. Accelerated solvent extraction ASE has been used for simultaneous extraction of organic compounds. The most favorable extraction conditions proved to be n hexane as the extraction solvent, temperature of 120 °C, pressure of 1500 psi and three static cycles in each case. Purification of the extract was accomplished by automated Power PrepTM/Sample Clean up system. The analyses were then performed by using gas chromatography coupled to triple quadrupole mass spectrometry. Utilizing triple quadruple mass spectrometry under positive EI with multiple reaction monitoring MRM mode, greatly enhances the sensitivity and selectivity of detection, compared to selective ion monitoring SIM mode. The GC QqQ MS/MS sensitivity, lower than that of GC HRMS, is good enough LODs in the down to low pg levels to detect the normal concentrations of these compounds in environmental samples. The obtained analytical results demonstrate excellent recoveries for the various congeners, comparable to those of official methods and detection limits useful for the analysis of real matrices. The determination of these compounds in soils and sediments and the evaluation of the distribution of various congeners fingerprint method has allowed to obtain information on the origin of the contamination. Published version XXVI Congresso Nazionale della Societa Chimica Italiana Paestum SA 10 14/09/2017 Internazionale Contributo Contributo in atti di convegno giuseppe.bagnuolo BAGNUOLO GIUSEPPE ruggiero.ciannarella CIANNARELLA RUGGIERO giuseppe.mascolo MASCOLO GIUSEPPE |
