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Efikasnost različitih metoda za određivanje ostataka organofosfata u fermentisanim uzorcima žita

dc.creatorĐorđević, Tijana
dc.creatorŠiler-Marinković, Slavica
dc.creatorĐurović-Pejčev, Rada
dc.creatorDimitrijević-Branković, Suzana
dc.creatorGajić-Umiljendić, Jelena
dc.date.accessioned2021-03-10T12:03:24Z
dc.date.available2021-03-10T12:03:24Z
dc.date.issued2013
dc.identifier.issn1820-3949
dc.identifier.urihttp://TechnoRep.tmf.bg.ac.rs/handle/123456789/2335
dc.description.abstractIn the present work, the efficiencies of three different sample preparation methods for GC/ MS determination of pirimiphos-methyl and chlorpyrifos-methyl residues in wheat (Triticum spelta) samples fermented by Lactobacillus plantarum were compared. All three methods were based on methanol:acetone=1:1 extraction, while further purification of the obtained samples was altered. First purification was through a column containing a mixture of aluminium oxide and activated charcoal slurry-packed and eluted with dichlormethane, the second was purification on a florisil column slurry-packed and eluted with ethyl acetate:acetone=4:1, while the third was based on a combination of the former two methods, i.e. clean-up through columns filled with a mixture of aluminum oxide and activated charcoal slurry-packed and eluted with ethyl acetate:acetone=4:1. The second method was found the most effective for obtaining satisfactory recoveries at four fortification levels. For pirimiphos-methyl, recoveries were in the range of 91.3-96.0% and had good reproducibility, i.e. RSD ranging from 2.2-4.1%, while the corresponding range for chlorpyrifos-methyl was 81.6-88.2%, and the RSD range 2.5-5.4%. The chosen method was further optimized in order to establish the optimum volume of elution solvent used during the clean-up procedures. The highest recoveries of 93.7±3.5% for pirimiphos-methyl and 85.3±2.5% for chlorpyrifos-methyl were obtained after elution with 25 ml volume of solvent. Considering all, simple, efficient and reliable GC/MS detection of pirimiphosmethyl and chlorpyrifos-methyl residues in wheat grain substrate altered by fermentation with L. plantarum was achieved by the two-steps extraction with 25 ml of methanol:acetone=1:1 solvent mix for 30 min, followed by a clean-up procedure through a glass column with florisil coupled with elution by 25 ml of ethyl acetate:acetone=4:1.en
dc.description.abstractPoređene su efikasnosti tri različite metode pripreme uzoraka za određivanje ostataka pirimifos-metila i hlorpirifos-metila u uzorcima pšenice (Triticum spelta) fermentisane sa Lactobacillus plantarum. Sve tri metode zasnivale su se na metanolsko-acetonskoj (1:1) ekstrakciji dok su se procedure prečišćavanja dobijenih ekstrakata razlikovale. Prva metoda bila je prečišćavanje kroz kolonu punjenu smešom aluminijum-oksida i aktivnog uglja u kombinaciji sa dihlormetanom kao eluentom, druga prečišćavanje kroz kolonu punjenu florisilom u kombinaciji sa smešom etil-acetata i acetona (4:1) kao eluentom, dok se treća zasnivala na kombinaciji prve dve, tj. prečišćavanju kroz kolonu punjenu smešom aluminijum-oksida i aktivnog uglja u kombinaciji sa smešom etil-acetata i acetona (4:1) kao eluentom. Druga testirana metoda pokazala se kao najefikasnija, pri čemu su dobijeni prinosi pirimifos-metila u opsegu 91,3-96,0% za četiri koncentraciona nivoa obogaćivanja, sa RSD% u opsegu 2,2-4,1%, dok su za hlorpirifos-metil ovi prinosi bili u opsegu 81,6-88,2% sa RSD% u opsegu 2,5-5,4%. Odabrana metoda je dodatno optimizovana variranjem različitih zapremina korišćenog eluenta. Najveći prinos metode za oba ispitivana pesticida postignut je pri zapremini eluenta od 25 ml (93,7±3.5% za pirimifos-metil i 85,3±2,5% za hlorpirifos-metil). Predložena metoda, bazirana na 30-minutnoj ekstrakciji sa 25 ml smeše metanol:aceton=1:1, prečišćavanju na florisilskoj koloni i eluiranju sa 25 ml smeše etilacetat: aceton=4:1, pokazala se kao efikasna, jednostavna i pouzdana metoda za određivanje ostataka ispitivanih organofosfata u fermentisanom žitnom supstratu.sr
dc.publisherInstitute of Pesticides and Environmental Protection
dc.relationinfo:eu-repo/grantAgreement/MESTD/Technological Development (TD or TR)/31043/RS//
dc.rightsopenAccess
dc.rights.urihttps://creativecommons.org/licenses/by-sa/4.0/
dc.sourcePesticidi i fitomedicina
dc.subjectmethod efficiencyen
dc.subjectpesticide determinationen
dc.subjectpirimiphos-methylen
dc.subjectchlorpyrifosmethylen
dc.subjectfermented wheaten
dc.subjectefikasnost metodesr
dc.subjectodređivanje pesticidasr
dc.subjectpirimifos-metilsr
dc.subjecthlorpirifos-metilsr
dc.subjectfermentisana pšenicasr
dc.titleEfficiencies of different methods for determination of organophosphate pesticide residues in fermented wheat substrateen
dc.titleEfikasnost različitih metoda za određivanje ostataka organofosfata u fermentisanim uzorcima žitasr
dc.typearticle
dc.rights.licenseBY-SA
dc.citation.epage140
dc.citation.issue2
dc.citation.other28(2): 133-140
dc.citation.rankM24
dc.citation.spage133
dc.citation.volume28
dc.identifier.doi10.2298/PIF1302133D
dc.identifier.fulltexthttp://TechnoRep.tmf.bg.ac.rs/bitstream/id/8965/1820-39491302133D.pdf
dc.type.versionpublishedVersion


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