Razvoj višekomponentnih kromatografskih metoda za određivanje ostataka pesticida u uzorcima čaja

doctoral thesis

• Title (english): Development of multicomponent chromatographic methods for determination of pesticide residues in tea samples
• Author: Antonija Beneta
• Mentor: Dragana Mutavdžić Pavlović (mentor)
• Committee member: Sandra Babić (predsjednik povjerenstva)
• Committee member: Svjetlana Krištafor (član povjerenstva)
• Committee member: Ines Primožič (član povjerenstva)
• Granter: University of Zagreb; Faculty of Chemical Engineering and Technology; Zagreb
• Defense date and country: 2018-12-06, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry; Analytic Chemistry
• Universal decimal classification (UDC): 54 - Chemistry. Crystallography. Mineralogy

Abstract

U ovom radu razvijena je metoda za određivanje 300 pesticida u uzorcima čaja i biljnih infuzija modificiranom QuEChERS metodom i plinskom kromatografijom vezanom sa spektrometrijom masa (GC-MS/MS). Razvijena metoda, koja se odlikovala brzinom, jednostavnošću i ekonomičnošću usprkos velikom broju analiziranih pesticida, potvrđena je u skladu s uputama iz dokumenta SANTE/11813/2017 te primjenjena u rutinskom radu. U tu svrhu prvo su optimizirani različiti GC i MS/MS parametri nakon čega se naglasak dao na modifikaciju izvorne QuEChERS metode koja je dizajnirana za uzorke s više od 75 % vode. Ukupno vrijeme trajanja analize tako razvijene metode je 28 minuta uz 0,6 μL volumena injektiranja. Razvijena metoda je validirana. Za točnu kvantifikaciju upotrijebljene su umjerne krivulje u matici (u rasponu od 10 μg/kg – 250 μg/kg) u svrhu kompenziranja utjecaja matice. Granice kvantitativnosti (LOQ) su u rasponu između 0,06 μg/kg i 135 μg/kg, a za većinu pesticida LOQ je ispod regulatornih maksimalno dozvoljenih količina. Većina iskorištenja za 10 μg/kg je u rasponu od 70- 120 % što ukazuje na zadovoljavajuću točnost metode. Validirana metoda primijenjena je u analizi komercijalnih čajeva i biljnih infuzija te je ustanovljena prisutnost klorpirifosa, DEET-a, tebukonazola, terbutilazina, piperonil-butoksida, bifenila, pendimetalina, pirimifos-metila i 4,4'-DDE-a u više od 100 uzoraka od ukupno 1466 analiziranih realnih uzoraka. Za navedene najčešće dokazane pesticide napravljen je izračun za procjenu rizika na ljudsko zdravlje.

Abstract (english)

A method for the determination of 300 pesticides in tea samples and plant infusions has been developed in this paper by modified QuEChERS method and gas chromatographic mass spectrometry (GC-MS/MS). The developed method, which was characterized by fast speed analysis, simplicity and economy despite a large number of analyzed pesticides, was confirmed in accordance with instructions from SANTE/11813/2017 and applied in routine work. For this purpose, GC and MS/MS parameters were optimized at the beginning and afterward emphasis being given to the modification of the original QuEChERS method, designed for samples with more than 75 % of water content. The total analysis runtime of developed method is 28 minutes with injection volume of 0.6 μL. The developed method is validated. Matrix-matched calibration curves were used for accurate quantification (ranging from 10 μg/kg to 250 μg/kg) to compensate the matrix effect. Limits of quantification (LOQs) are in range between 0.06 μg/kg and 135 μg/kg, and for most pesticides, LOQ is below the regulatory maximum residue level. Most of recoveries for 10 μg/kg range from 70 to 120 % which indicates satisfactory method accuracy. The validated method was applied to analysis of commercial tea samples and herbal infusions and the presence of chlorpyrifos, DEET, tebuconazole, terbuthylazine, piperonyl butoxide, biphenyls, pendimethalins, pirimiphos-methyl and 4,4'-DDE was found in more than 100 samples of total 1466 analyzed real samples. For these most commonly proven pesticides, calculation of human health risk assessment was calculated.

• Keywords: višekomponentna metoda; pesticidi; čaj i biljne infuzije; plinska kromatografija vezana sa spektrometrijom masa; procjena rizika
• Keywords (english): multicomponent method; pesticides; tea and herbal infusions; gas chromatography - tandem mass spectrometry; risk assessment
• Language: croatian
• URN:NBN: urn:nbn:hr:149:945842
• Promotion: 2018
• Study programme: Title: Engineering Chemistry - Doctoral Course; 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: 152 str. ; 30 cm
• File origin: Born digital
• Access conditions: Open access
• Created on: 2023-08-29 08:49:31