Efficiencies of Different Methods for Determination of Organophosphate Pesticide Residues in Fermented Wheat Substrate
Efikasnost različitih metoda za određivanje ostataka organofosfata u fermentisanim uzorcima žita
dc.contributor.author | Djordjevic, Tijana | |
dc.contributor.author | Siler-Marinkovic, Slavica | |
dc.contributor.author | Djurovic-Pejcev, Rada | |
dc.contributor.author | Dimitrijevic-Brankovic, Suzana | |
dc.contributor.author | Gajic Umiljendic, Jelena | |
dc.date.accessioned | 2015-11-08T16:16:48Z | |
dc.date.available | 2015-11-08T16:16:48Z | |
dc.identifier.uri | http://arhiva.nara.ac.rs/handle/123456789/1472 | |
dc.description.abstract | In 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.abstract | Poređene 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.subject | Method efficiency | en |
dc.subject | Pesticide determination | en |
dc.subject | Pirimiphos-methyl | en |
dc.subject | Chlorpyrifosmethyl | sr |
dc.subject | Fermented wheat | en |
dc.subject | Efikasnost metode | sr |
dc.subject | određivanje pesticida | sr |
dc.subject | pirimifos-metil | sr |
dc.subject | hlorpirifos-metil | sr |
dc.subject | fermentisana pšenica | sr |
dc.title | Efficiencies of Different Methods for Determination of Organophosphate Pesticide Residues in Fermented Wheat Substrate | en |
dc.title.alternative | Efikasnost različitih metoda za određivanje ostataka organofosfata u fermentisanim uzorcima žita | sr |
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VOL 28 *No.2
http://www.pesting.org.rs/2013.php