Mikroekstrakcija u čvrstoj fazi - uzorkovanje iz gasovite faze u određivanju ostataka pesticida - 1. optimizacija uslova ekstrakcije
Headspace solid phase microextraction in pesticide residues analysis: 1. Optimization of extraction conditions
Апстракт
Metoda mikroekstrakcije u čvrstoj fazi - uzorkovanje iz gasovite faze (HS/SPME) je uspešno primenjena za istovremenu višekomponentnu analizu heksahlorobenzena (HCB), teflutrina, heptahlora, aldrina, hlorpirifosa, fentiona i bifentrina u vodenoj sredini. U radu je korišćeno nepolarno polidimetilsiloksansko vlakno (PDMS). Detekcija i kvantifikacija analita je vršena metodom gasno-masene spektrometrije (GC/MS). Optimalni uslovi HS/SPME metode su određeni praćenjem efikasnosti ekstrakcije na različitim temperaturama, odnosno u funkciji vremena na konstantnoj temperaturi. Za svaki ispitivani pesticid, određena je optimalna temperatura ekstrakcije: 60°C za HCB i heptahlor, 80°C za aldrin, hlorpirifos, fention i teflutrin, temperatura veća od 80°C za bifentrin. Za ispitivanu smešu, temperatura od 60°C je izabrana za praktičan rad. Na osnovu dobijenih vremenskih profila, utvrđeno je da se dobra osetljivost metode postiže i kada se radi sa vremenom ekstrakcije kraćim od ravnotežnog. Ovaj zaklju...čak je potvrđen i eksperimentalno dobijenim koncentracionim profilima, pri čemu su dobijeni sledeći opsezi linearnosti: 0.05- 10 ng/ml (HCB), 0.05-25 ng/ml (teflutrin), 0.05-40 ng/ml (heptahlor), 0.05-40 ng/ml (aldrin), 0.05-25 ng/ml (hlorpirifos), 0.05-25 ng/ml (fention) i 0.05-25 ng/ml (bifentrin). Relativne standardne devijacije (RSD) računate na osnovu tri ponovljena merenja su uvek bile manje od 15%.
The method of headspace solid phase microextraction (HS/SPME) was successfully used in a simultaneous multicomponent analysis of hexachlorobenzene (HCB), tefluthrin, heptachlor, aldrin, chlorpyrifos, fenthion and bifenthrin in aqueous medium. Measurements were performed using a nonpolar polydimethyl siloxane (PDMS) fiber. Detection and quantification
were done by gas chromatography/mass spectrometry (GC/MS).
Optimal conditions for HS/SPME were determined both by performing extraction at different temperatures and examining extraction time profiles at constant temperature. Optimal extraction temperature for each pesticide studied was determined as follows: 60°C for HCB and for heptachlor, 80°C for aldrin and for chlorpyrifos, fenthion and tefluthrin, and temperature exceeding 80°C for bifenthrin. For the pesticide mixture studied, 60°C was identified as the optimum extraction temperature. Based on the time profiles obtained, it was confirmed that satisfactory extraction sensitivity can ...be obtained even for extraction times shorter than the time required to reach a sorption equilibrium. This conclusion was confirmed by linear concentration profiles obtained for the following ranges: 0.05-10 ng/ml (HCB), 0.05-25 ng/ml (tefluthrin), 0.05-40 ng/ml (heptachlor), 0.05-40 ng/ml (aldrin), 0.05-25 ng/ml (chlorpyrifos), 0.05-25 ng/ml (fenthion) and 0.05-25 ng/ml (bifenthrin). Relative standard deviation (RSD) values for triplicate measurements did not exceed 15%.
Кључне речи:
ostaci pesticida / optimizacija / HS/SPME / pesticide residues / optimisation / HS/SPMEИзвор:
Pesticidi i fitomedicina, 2007, 22, 1, 65-70Издавач:
- Institut za pesticide i zaštitu životne sredine, Beograd i Društvo za zaštitu bilja Srbije, Beograd
Институција
Institut za pesticide i zaštitu životne sredineTY - JOUR AU - Đurović, Rada AU - Milinović, Jelena AU - Marković, Mirjana AU - Marković, Dragan PY - 2007 UR - https://ripest.pesting.org.rs/handle/123456789/56 AB - Metoda mikroekstrakcije u čvrstoj fazi - uzorkovanje iz gasovite faze (HS/SPME) je uspešno primenjena za istovremenu višekomponentnu analizu heksahlorobenzena (HCB), teflutrina, heptahlora, aldrina, hlorpirifosa, fentiona i bifentrina u vodenoj sredini. U radu je korišćeno nepolarno polidimetilsiloksansko vlakno (PDMS). Detekcija i kvantifikacija analita je vršena metodom gasno-masene spektrometrije (GC/MS). Optimalni uslovi HS/SPME metode su određeni praćenjem efikasnosti ekstrakcije na različitim temperaturama, odnosno u funkciji vremena na konstantnoj temperaturi. Za svaki ispitivani pesticid, određena je optimalna temperatura ekstrakcije: 60°C za HCB i heptahlor, 80°C za aldrin, hlorpirifos, fention i teflutrin, temperatura veća od 80°C za bifentrin. Za ispitivanu smešu, temperatura od 60°C je izabrana za praktičan rad. Na osnovu dobijenih vremenskih profila, utvrđeno je da se dobra osetljivost metode postiže i kada se radi sa vremenom ekstrakcije kraćim od ravnotežnog. Ovaj zaključak je potvrđen i eksperimentalno dobijenim koncentracionim profilima, pri čemu su dobijeni sledeći opsezi linearnosti: 0.05- 10 ng/ml (HCB), 0.05-25 ng/ml (teflutrin), 0.05-40 ng/ml (heptahlor), 0.05-40 ng/ml (aldrin), 0.05-25 ng/ml (hlorpirifos), 0.05-25 ng/ml (fention) i 0.05-25 ng/ml (bifentrin). Relativne standardne devijacije (RSD) računate na osnovu tri ponovljena merenja su uvek bile manje od 15%. AB - The method of headspace solid phase microextraction (HS/SPME) was successfully used in a simultaneous multicomponent analysis of hexachlorobenzene (HCB), tefluthrin, heptachlor, aldrin, chlorpyrifos, fenthion and bifenthrin in aqueous medium. Measurements were performed using a nonpolar polydimethyl siloxane (PDMS) fiber. Detection and quantification were done by gas chromatography/mass spectrometry (GC/MS). Optimal conditions for HS/SPME were determined both by performing extraction at different temperatures and examining extraction time profiles at constant temperature. Optimal extraction temperature for each pesticide studied was determined as follows: 60°C for HCB and for heptachlor, 80°C for aldrin and for chlorpyrifos, fenthion and tefluthrin, and temperature exceeding 80°C for bifenthrin. For the pesticide mixture studied, 60°C was identified as the optimum extraction temperature. Based on the time profiles obtained, it was confirmed that satisfactory extraction sensitivity can be obtained even for extraction times shorter than the time required to reach a sorption equilibrium. This conclusion was confirmed by linear concentration profiles obtained for the following ranges: 0.05-10 ng/ml (HCB), 0.05-25 ng/ml (tefluthrin), 0.05-40 ng/ml (heptachlor), 0.05-40 ng/ml (aldrin), 0.05-25 ng/ml (chlorpyrifos), 0.05-25 ng/ml (fenthion) and 0.05-25 ng/ml (bifenthrin). Relative standard deviation (RSD) values for triplicate measurements did not exceed 15%. PB - Institut za pesticide i zaštitu životne sredine, Beograd i Društvo za zaštitu bilja Srbije, Beograd T2 - Pesticidi i fitomedicina T1 - Mikroekstrakcija u čvrstoj fazi - uzorkovanje iz gasovite faze u određivanju ostataka pesticida - 1. optimizacija uslova ekstrakcije T1 - Headspace solid phase microextraction in pesticide residues analysis: 1. Optimization of extraction conditions EP - 70 IS - 1 SP - 65 VL - 22 UR - conv_22 ER -
@article{ author = "Đurović, Rada and Milinović, Jelena and Marković, Mirjana and Marković, Dragan", year = "2007", abstract = "Metoda mikroekstrakcije u čvrstoj fazi - uzorkovanje iz gasovite faze (HS/SPME) je uspešno primenjena za istovremenu višekomponentnu analizu heksahlorobenzena (HCB), teflutrina, heptahlora, aldrina, hlorpirifosa, fentiona i bifentrina u vodenoj sredini. U radu je korišćeno nepolarno polidimetilsiloksansko vlakno (PDMS). Detekcija i kvantifikacija analita je vršena metodom gasno-masene spektrometrije (GC/MS). Optimalni uslovi HS/SPME metode su određeni praćenjem efikasnosti ekstrakcije na različitim temperaturama, odnosno u funkciji vremena na konstantnoj temperaturi. Za svaki ispitivani pesticid, određena je optimalna temperatura ekstrakcije: 60°C za HCB i heptahlor, 80°C za aldrin, hlorpirifos, fention i teflutrin, temperatura veća od 80°C za bifentrin. Za ispitivanu smešu, temperatura od 60°C je izabrana za praktičan rad. Na osnovu dobijenih vremenskih profila, utvrđeno je da se dobra osetljivost metode postiže i kada se radi sa vremenom ekstrakcije kraćim od ravnotežnog. Ovaj zaključak je potvrđen i eksperimentalno dobijenim koncentracionim profilima, pri čemu su dobijeni sledeći opsezi linearnosti: 0.05- 10 ng/ml (HCB), 0.05-25 ng/ml (teflutrin), 0.05-40 ng/ml (heptahlor), 0.05-40 ng/ml (aldrin), 0.05-25 ng/ml (hlorpirifos), 0.05-25 ng/ml (fention) i 0.05-25 ng/ml (bifentrin). Relativne standardne devijacije (RSD) računate na osnovu tri ponovljena merenja su uvek bile manje od 15%., The method of headspace solid phase microextraction (HS/SPME) was successfully used in a simultaneous multicomponent analysis of hexachlorobenzene (HCB), tefluthrin, heptachlor, aldrin, chlorpyrifos, fenthion and bifenthrin in aqueous medium. Measurements were performed using a nonpolar polydimethyl siloxane (PDMS) fiber. Detection and quantification were done by gas chromatography/mass spectrometry (GC/MS). Optimal conditions for HS/SPME were determined both by performing extraction at different temperatures and examining extraction time profiles at constant temperature. Optimal extraction temperature for each pesticide studied was determined as follows: 60°C for HCB and for heptachlor, 80°C for aldrin and for chlorpyrifos, fenthion and tefluthrin, and temperature exceeding 80°C for bifenthrin. For the pesticide mixture studied, 60°C was identified as the optimum extraction temperature. Based on the time profiles obtained, it was confirmed that satisfactory extraction sensitivity can be obtained even for extraction times shorter than the time required to reach a sorption equilibrium. This conclusion was confirmed by linear concentration profiles obtained for the following ranges: 0.05-10 ng/ml (HCB), 0.05-25 ng/ml (tefluthrin), 0.05-40 ng/ml (heptachlor), 0.05-40 ng/ml (aldrin), 0.05-25 ng/ml (chlorpyrifos), 0.05-25 ng/ml (fenthion) and 0.05-25 ng/ml (bifenthrin). Relative standard deviation (RSD) values for triplicate measurements did not exceed 15%.", publisher = "Institut za pesticide i zaštitu životne sredine, Beograd i Društvo za zaštitu bilja Srbije, Beograd", journal = "Pesticidi i fitomedicina", title = "Mikroekstrakcija u čvrstoj fazi - uzorkovanje iz gasovite faze u određivanju ostataka pesticida - 1. optimizacija uslova ekstrakcije, Headspace solid phase microextraction in pesticide residues analysis: 1. Optimization of extraction conditions", pages = "70-65", number = "1", volume = "22", url = "conv_22" }
Đurović, R., Milinović, J., Marković, M.,& Marković, D.. (2007). Mikroekstrakcija u čvrstoj fazi - uzorkovanje iz gasovite faze u određivanju ostataka pesticida - 1. optimizacija uslova ekstrakcije. in Pesticidi i fitomedicina Institut za pesticide i zaštitu životne sredine, Beograd i Društvo za zaštitu bilja Srbije, Beograd., 22(1), 65-70. conv_22
Đurović R, Milinović J, Marković M, Marković D. Mikroekstrakcija u čvrstoj fazi - uzorkovanje iz gasovite faze u određivanju ostataka pesticida - 1. optimizacija uslova ekstrakcije. in Pesticidi i fitomedicina. 2007;22(1):65-70. conv_22 .
Đurović, Rada, Milinović, Jelena, Marković, Mirjana, Marković, Dragan, "Mikroekstrakcija u čvrstoj fazi - uzorkovanje iz gasovite faze u određivanju ostataka pesticida - 1. optimizacija uslova ekstrakcije" in Pesticidi i fitomedicina, 22, no. 1 (2007):65-70, conv_22 .