University of Zagreb. Faculty of Science. Department of Chemistry.
Abstract
Razrađeni su postupci mikrovalne ili ultrazvučne ekstrakcije za multirezidualnu analizu tragova organoklorovih (OC) pesticida i specifičnih kongenera polikloriranih bifenila u tlu (35 spojeva) i u frakciji lebdećih čestica PM2,5 u zraku (27 spojeva). Otapalo za ekstrakciju bila je smjesa (n-heksan, aceton)=1:1. Pročišćeni ekstrakti analizirani su plinskom kromatografijom uz detekciju spojeva detektorom zahvata elektrona i spektrometrijom masa. Istražen je utjecaj sastojaka matrice tla na djelotvornost dvaju različitih postupaka ekstrakcije i selektivnost i osjetljivost odziva detektora. Mikrovalna ekstrakcija primijenjena je za analizu OC spojeva u tlima i jezerskim sedimentima skupljenim na području Nacionalnog parka Plitvička jezera te tlima skupljenim na području grada Varaždina, a ultrazvučna za analizu istih zagađivala u lebdećim česticama PM2,5 skupljenim u Zagrebu. Maseni udjeli OC zagađivala u tlu i sedimentima (ng kg-1 do g kg-1) kao i njihove masene koncentracije u česticama u zraku (pg m3) bili su na razini globalnog onečišćenja okoliša. U uzorcima tla i sedimenata najčešće je detektiran p,p'-DDE, a u česticama PM2,5 u zraku -heksaklorcikloheksan. Omjeri p,p'-DDE/p,p'-DDT u varaždinskim tlima i u lebdećim česticama u zraku upućuju na stalni unos tragova p,p'-DDT-a u okoliš. Masene koncentracije OC zagađivala u česticama PM2,5 u zraku bile su 2010. godine znatno niže od onih izmjerenih na istoj lokaciji u razdoblju od 2000. do 2003. godine.Abstract Microwave-assisted or ultrasound-assisted extraction procedures were developed for multiresidue trace analysis of organochlorine (OC) pesticides and specific polychlorinated biphenyl congeners in soil (35 compounds) and atmospheric particles PM2.5 (27 compounds). The extraction solvent was the mixture (n-hexane, acetone)=1:1. Purified extracts were analysed using gas chromatography with electron capture and mass spectrometric detection. The influence of soil matrix components on the efficiency of two different extraction procedures and on the selectivity and sensitivity of detector response was investigated. The microwave-assisted extraction was applied for the analysis of OC compounds in soils and lake sediments collected in the area of Plitvice Lakes National Park and in soils collected in the city of Varaždin, while the ultrasonic extraction was used for analyses of these pollutants in PM2.5 atmospheric particles collected in Zagreb. Mass fractions of OC pollutants in soils and sediments (ng kg-1 to g kg-1) as well as their mass concentrations in particles in air (pg m3) were at levels of global environmental pollution. The most frequently detected OC pollutant in soils and sediments was p,p'-DDE, and in PM2,5 particles in air -hexachlorocyclohexane. The p,p-DDE/p,p-DDT in Varaždin soils and in atmospheric particles indicated a constant input of p,p-DDT traces in the environment. Mass concentrations of OC pollutants in PM2.5 particles in air were considerably lower in 2010 than those measured at the same location in the 2000 to 2003 period
