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
Аутори
Đorđević, TijanaŠiler-Marinković, Slavica
Đurović-Pejčev, Rada
Dimitrijević-Branković, Suzana
Gajić-Umiljendić, Jelena
Чланак у часопису (Објављена верзија)
Метаподаци
Приказ свих података о документуАпстракт
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, recoveri...es 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.
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.
Кључне речи:
method efficiency / pesticide determination / pirimiphos-methyl / chlorpyrifosmethyl / fermented wheat / efikasnost metode / određivanje pesticida / pirimifos-metil / hlorpirifos-metil / fermentisana pšenicaИзвор:
Pesticidi i fitomedicina, 2013, 28, 2, 133-140Издавач:
- Institute of Pesticides and Environmental Protection
Финансирање / пројекти:
Институција/група
Tehnološko-metalurški fakultetTY - JOUR AU - Đorđević, Tijana AU - Šiler-Marinković, Slavica AU - Đurović-Pejčev, Rada AU - Dimitrijević-Branković, Suzana AU - Gajić-Umiljendić, Jelena PY - 2013 UR - http://TechnoRep.tmf.bg.ac.rs/handle/123456789/2335 AB - 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. AB - 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. PB - Institute of Pesticides and Environmental Protection T2 - Pesticidi i fitomedicina T1 - Efficiencies of different methods for determination of organophosphate pesticide residues in fermented wheat substrate T1 - Efikasnost različitih metoda za određivanje ostataka organofosfata u fermentisanim uzorcima žita EP - 140 IS - 2 SP - 133 VL - 28 DO - 10.2298/PIF1302133D ER -
@article{ author = "Đorđević, Tijana and Šiler-Marinković, Slavica and Đurović-Pejčev, Rada and Dimitrijević-Branković, Suzana and Gajić-Umiljendić, Jelena", year = "2013", 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., 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.", publisher = "Institute of Pesticides and Environmental Protection", journal = "Pesticidi i fitomedicina", title = "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", pages = "140-133", number = "2", volume = "28", doi = "10.2298/PIF1302133D" }
Đorđević, T., Šiler-Marinković, S., Đurović-Pejčev, R., Dimitrijević-Branković, S.,& Gajić-Umiljendić, J.. (2013). Efficiencies of different methods for determination of organophosphate pesticide residues in fermented wheat substrate. in Pesticidi i fitomedicina Institute of Pesticides and Environmental Protection., 28(2), 133-140. https://doi.org/10.2298/PIF1302133D
Đorđević T, Šiler-Marinković S, Đurović-Pejčev R, Dimitrijević-Branković S, Gajić-Umiljendić J. Efficiencies of different methods for determination of organophosphate pesticide residues in fermented wheat substrate. in Pesticidi i fitomedicina. 2013;28(2):133-140. doi:10.2298/PIF1302133D .
Đorđević, Tijana, Šiler-Marinković, Slavica, Đurović-Pejčev, Rada, Dimitrijević-Branković, Suzana, Gajić-Umiljendić, Jelena, "Efficiencies of different methods for determination of organophosphate pesticide residues in fermented wheat substrate" in Pesticidi i fitomedicina, 28, no. 2 (2013):133-140, https://doi.org/10.2298/PIF1302133D . .