Abstract :
[en] This thesis focused on the development and validation of analytical methods for the de-tection and quantification of Persistent Organic Pollutants (POPs) in biological matrices, namely food and feed samples. POPs are a group of chemical compounds listed after the Stockholm Convention in 2001, with demonstrated toxicity and dangerousness for envi-ronment, animals and humans.
In this work of thesis, special attention was reserved to some selected POPs: polychlo-rodibenzo-p-dioxins (PCDDs), polychlorodibenzofurans (PCDFs), usually referred to as “dioxins”, and polychlorinated biphenyls (PCBs), as there is a big concern about these contaminants in Taranto, a city in the Southern Italy very close to Bari, my home town. Taranto, indeed, is characterized by a large industrial area with a steel mill, several incin-erators and a refinery in few kilometre radius (Di Leo et al., 2014). This work has been done in collaboration with the University of Liège (Belgium) where a consolidated exper-tise in the field of POP measurements was available, especially in terms of dioxin anal-yses.
In Chapter 1 the main steps, from sample preparation to data elaboration, of a validated confirmatory method for dioxin and PCB detection in food and feed using gas chromatog-raphy coupled to tandem mass spectrometry Triple Quad instrument (GC-MS/MS Triple Quad) have been described. This method was developed at the University of Liège in the framework of the last updates of the EU Regulation that in 2014 allowed confirmatory quantitative analysis of dioxins with Triple Quad. This method was the starting point of this work of thesis, because it was used for all dioxin and PCB quantifications. In Chapter 2 and chapter 3 alternative clean-up approaches for dioxin analysis in fatty food matrices have been developed using different automated systems. These works have been done in the framework of solvent and time saving for high throughput analytical methods in dioxin analysis. In chapter 2, an already existing automated system, DEXTechTM from LCTech GmbH (LCTech GmbH, Bahnweg 41, 84405 Dorfen, Germany) was used for sample clean-up, but a completely new clean-up approach was developed with this. GC-MS/MS Triple Quad instrument, as well as Magnetic Sector High Resolution Mass Spectrometry (HRMS) instrument were employed for final quantification, to demonstrate the suitability of our newly developed clean-up approaches whatever the instrumental detection. In Chapter 3 PowerPrepTM automated system from Fluid Management System (FMS Inc., 580 Pleasant Street, Watertown, MA 02472, USA) was used and our routine sample clean-up approach was modified in order to enhance the efficiency and to reduce cost and solvent consumption of the analysis. In Chapter 4 the main method for dioxin analysis was adapted for the integration of Dechloranes in the list of the analytes targeted in the regular control for dioxins in food and feed. Dechloranes are a family of 6 organo-chlorinated compounds with structure similar to Mirex, also called Dechlorane, a POP listed in the Stockholm convention. Dechloranes have been found in human blood of people from Europe (Brasseur et al., 2014) and in this work an analytical method for Dechlorane detection was developed and validated to investigate food as a possible route of exposure for humans in Europe, where no production plant has been identified so far. The analytical method was used to analyse 88 food and feed real sample and to give an idea of Dechlorane daily dietary intake.
