Razvoj multirezidualne metode za određivanje pesticida u vinima vezanim sustavom plinska kromatografija-spektrometrija masa

doctoral thesis

• Title (english): Development of multiresidue method for the determination of pesticides in wine by gas chromatography-mass spectrometry
• Author: Maja Pelajić
• Mentor: Dubravka Vitali Čepo (mentor); MBZ: 257935
• Committee member: Vlasta Drevenkar (predsjednik povjerenstva)
• Committee member: Dubravka Vitali Čepo (član povjerenstva); MBZ: 257935
• Committee member: Dragana Mutavdžić Pavlović (član povjerenstva); MBZ: 236333
• Granter: University of Zagreb; Faculty of Science; (Department of Chemistry); Zagreb
• Defense date and country: 2016-05-20, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry
• Universal decimal classification (UDC): 54 - Chemistry. Crystallography. Mineralogy

Abstract

Razvijena je multirezidualna metoda za određivanje 25 pesticida u vinima plinskom kromatografijom vezanom sa spektrometrijom masa. Optimirana je ekstrakcija na čvrstoj fazi uz sorbens OASIS HLB te postupak ekstrakcije QuEChERS s težištem na optimizaciji koncentracije dodanih soli radi podešavanja raspodjele analita između dviju faza. Za svaki postupak priprave uzorka provedena je validacija za crno i bijelo vino kao dvije zasebne matrice uzorka. Granice određivanja pesticida za oba postupka bile su u rasponu od 0,01 g L1 do 250 g L-1. Preciznost, izražena kao relativna standardna devijacija, bila je <20 %, dok je točnost, izražena kao analitički povrat, za većinu pesticida bila u rasponu od 70 % do 120 %. Ispitan je utjecaj matrice na određivanje pesticida pri čemu je izračunata djelotvornost postupaka priprave uzorka. U okviru validacije metoda procijenjena je mjerna nesigurnost koja je bila <50 % za većinu pesticida. Predloženim analitičkim postupcima analizirana su 63 uzorka različitih vina da bi se dobio prvi uvid u koncentracije ostataka pesticida u vinima s područja Hrvatske.

Abstract (english)

A new multiresidue method was developed for determination of 25 pesticides in wines by gas chromatography mass spectrometry. Two sample preparation procedures were optimized; solid phase extraction using OASIS HLB and QuEChERS procedure, where salt concentrations were optimised in order to adjust the distribution of pesticides between two immiscible phases. Method validation, including uncertainty estimation (<50 % for most pesticides), was performed independently for red and white wine as two different matrices and for each sample preparation procedure. Limits of quantification were between 0,01 g L-1 and 250 g L-1. The recoveries of most pesticides were between 70 % and 120 % with relative standard deviations <20 %. The matrix effect was investigated and the quality of sample preparation procedures has been evaluated in terms of extraction efficiency. The proposed analytical procedures were applied to 63 Croatian wine samples of different varieties in order to provide the first insight into pesticide residue concentrations in Croatian wines.

• Keywords: ekstrakcija na čvrstoj fazi; plinska kromatografija vezana sa spektrometrijom masa; pesticidi; QuEChERS; vina
• Keywords (english): gas chromatography-mass spectrometry; pesticides; QuEChERS; solid phase extraction; wines
• Language: croatian
• URN:NBN: urn:nbn:hr:217:553837
• Study programme: Title: Doctoral study in chemistry; Study programme type: university; Study level: postgraduate; Academic / professional title: doktor/doktorica znanosti, područje prirodnih znanosti, polje kemija (doktor/doktorica znanosti, područje prirodnih znanosti, polje kemija)
• Type of resource: Text
• Extent: 203 str. ; 30 cm
• File origin: Born digital
• Access conditions: Open access
• Created on: 2017-02-06 10:35:18