Application of liquid chromatography with diode-array detector for determination of acetamiprid and 6-chloronicotinic acid residues in sweet cherry samples
Primena tečne hromatografije sa DAD detektorom za određivanje ostataka acetamiprida i 6-hlornikotinske kiseline u uzorcima trešanja
2012
Аутори
Lazić, SanjaŠunjka, Dragana B.
Grahovac, Nada
Guzsvány, Valéria
Bagi, Ferenc
Budakov, Dragana
Чланак у часопису (Објављена верзија)
Метаподаци
Приказ свих података о документуАпстракт
A rapid and simple method for simultaneous determination of acetamiprid and its metabolite 6-chloronicotinic acid in sweet cherry samples has been developed. This residue analysis method is based on the reversed phase separation on C18 column with gradient elution. Analytes' determination and quantification were performed by high performance liquid chromatography (HPLC) with diode-array detector and chromatograms were extracted at 230 nm. Extraction efficiency experiments demonstrated the ability of this method to extract neonicotinoids from sweet cherry samples. These insecticides were extracted with a mixture of acetonitril/0.1N ammonium-chloride (8/2, v/v). The average recoveries of acetamiprid and 6-chlornicotinic acid from sweet cherry samples were in the range of 95-101% and 73-83%, respectively, with the associated relative standard deviations (RSDs) lt 5%. Expanded measurement uncertainties for the analyzed compounds were 2.7 and 3.01%. The limit of quantification (LOQ) was 10... μg/kg and 30 μg/kg for acetamiprid and 6-chloronicotinic acid, respectively. Thus, the developed HPLC/DAD method can be considered a useful tool for sensitive and rapid determination of acetamiprid and 6-chloronicotinic acid. Hence, the method may find further application in the analysis of real sweet cherry samples contaminated with these insecticides at a ppb level.
U radu je predstavljena jednostavna metoda za određivanje acetamiprida i njegovog metabolita, 6-hlornikotinske kiseline, u uzorcima trešanja. Metoda je bazirana na primeni reverzno-faznog razdvajanja na C18 koloni primenom gradijentnog eluiranja. Određivanje i kvantifikacija analita je vršena tečnom hromatografijom (HPLC) sa DAD detektorom, pri čemu je korišćena talasna dužina od 230 nm. Tačnost metode je ocenjena procenom merne nesigurnosti. Ekstrakcija acetamiprida i 6-hlornikotinske kiseline iz uzoraka trešanja je vršena smešom acetonitril/amonijum-hlorid (0,1N) u odnosu 80:20 (v/v). Sva merenja su vršena u tri ponavljanja, pri čemu su dobijeni prinosi određivanja acetamiprida i 6-hlornikotinske kiseline u rasponima 95-101% i 73-83%, respektivno. Relativne standardne devijacije (RSD) merenja su u svim slučajevima bile ispod 5%. Limiti kvantifikacije za acetamiprid i 6-HNK iznosili su 10 i 30 μg/kg, respektivno. Kombinovana merna nesigurnost rezultata analize acetamiprida i njegovog ...metabolita procenjena je na 1,35, odnosno 1,50%, a proširena na 2,7 i 3,01%, upotrebom faktora pokrivanja (k=2) koji odgovara nivou poverenja od 95%, za normalnu raspodelu. Nakon validacije i procene merne neizvesnosti dobijeni rezultati pokazuju da se razvijena HPLC/DAD metoda može primeniti za određivanje sadržaja acetamiprida i 6-hlornikotinske kiseline u uzorcima trešanja i relevantnim matriksima kontaminiranim ovim jedinjenjima.
Кључне речи:
acetamiprid / 6-chloronicotinic acid / HPLC/DAD / sweet cherry / pesticide residues / acetamiprid / 6-hlornikotinska kiselina / HPLC/DAD / trešnje / ostaci pesticidaИзвор:
Pesticidi i fitomedicina, 2012, 27, 4, 321-329Издавач:
- Institut za pesticide i zaštitu životne sredine, Beograd i Društvo za zaštitu bilja Srbije, Beograd
Финансирање / пројекти:
- Стварање слабобујних подлога за трешњу и вишњу и развијање интензивне технологије гајења на принципима одрживе пољопривреде (RS-MESTD-Technological Development (TD or TR)-31038)
Колекције
Институција/група
FiVeRTY - JOUR AU - Lazić, Sanja AU - Šunjka, Dragana B. AU - Grahovac, Nada AU - Guzsvány, Valéria AU - Bagi, Ferenc AU - Budakov, Dragana PY - 2012 UR - http://fiver.ifvcns.rs/handle/123456789/1131 AB - A rapid and simple method for simultaneous determination of acetamiprid and its metabolite 6-chloronicotinic acid in sweet cherry samples has been developed. This residue analysis method is based on the reversed phase separation on C18 column with gradient elution. Analytes' determination and quantification were performed by high performance liquid chromatography (HPLC) with diode-array detector and chromatograms were extracted at 230 nm. Extraction efficiency experiments demonstrated the ability of this method to extract neonicotinoids from sweet cherry samples. These insecticides were extracted with a mixture of acetonitril/0.1N ammonium-chloride (8/2, v/v). The average recoveries of acetamiprid and 6-chlornicotinic acid from sweet cherry samples were in the range of 95-101% and 73-83%, respectively, with the associated relative standard deviations (RSDs) lt 5%. Expanded measurement uncertainties for the analyzed compounds were 2.7 and 3.01%. The limit of quantification (LOQ) was 10 μg/kg and 30 μg/kg for acetamiprid and 6-chloronicotinic acid, respectively. Thus, the developed HPLC/DAD method can be considered a useful tool for sensitive and rapid determination of acetamiprid and 6-chloronicotinic acid. Hence, the method may find further application in the analysis of real sweet cherry samples contaminated with these insecticides at a ppb level. AB - U radu je predstavljena jednostavna metoda za određivanje acetamiprida i njegovog metabolita, 6-hlornikotinske kiseline, u uzorcima trešanja. Metoda je bazirana na primeni reverzno-faznog razdvajanja na C18 koloni primenom gradijentnog eluiranja. Određivanje i kvantifikacija analita je vršena tečnom hromatografijom (HPLC) sa DAD detektorom, pri čemu je korišćena talasna dužina od 230 nm. Tačnost metode je ocenjena procenom merne nesigurnosti. Ekstrakcija acetamiprida i 6-hlornikotinske kiseline iz uzoraka trešanja je vršena smešom acetonitril/amonijum-hlorid (0,1N) u odnosu 80:20 (v/v). Sva merenja su vršena u tri ponavljanja, pri čemu su dobijeni prinosi određivanja acetamiprida i 6-hlornikotinske kiseline u rasponima 95-101% i 73-83%, respektivno. Relativne standardne devijacije (RSD) merenja su u svim slučajevima bile ispod 5%. Limiti kvantifikacije za acetamiprid i 6-HNK iznosili su 10 i 30 μg/kg, respektivno. Kombinovana merna nesigurnost rezultata analize acetamiprida i njegovog metabolita procenjena je na 1,35, odnosno 1,50%, a proširena na 2,7 i 3,01%, upotrebom faktora pokrivanja (k=2) koji odgovara nivou poverenja od 95%, za normalnu raspodelu. Nakon validacije i procene merne neizvesnosti dobijeni rezultati pokazuju da se razvijena HPLC/DAD metoda može primeniti za određivanje sadržaja acetamiprida i 6-hlornikotinske kiseline u uzorcima trešanja i relevantnim matriksima kontaminiranim ovim jedinjenjima. PB - Institut za pesticide i zaštitu životne sredine, Beograd i Društvo za zaštitu bilja Srbije, Beograd T2 - Pesticidi i fitomedicina T1 - Application of liquid chromatography with diode-array detector for determination of acetamiprid and 6-chloronicotinic acid residues in sweet cherry samples T1 - Primena tečne hromatografije sa DAD detektorom za određivanje ostataka acetamiprida i 6-hlornikotinske kiseline u uzorcima trešanja EP - 329 IS - 4 SP - 321 VL - 27 DO - 10.2298/PIF1204321L ER -
@article{ author = "Lazić, Sanja and Šunjka, Dragana B. and Grahovac, Nada and Guzsvány, Valéria and Bagi, Ferenc and Budakov, Dragana", year = "2012", abstract = "A rapid and simple method for simultaneous determination of acetamiprid and its metabolite 6-chloronicotinic acid in sweet cherry samples has been developed. This residue analysis method is based on the reversed phase separation on C18 column with gradient elution. Analytes' determination and quantification were performed by high performance liquid chromatography (HPLC) with diode-array detector and chromatograms were extracted at 230 nm. Extraction efficiency experiments demonstrated the ability of this method to extract neonicotinoids from sweet cherry samples. These insecticides were extracted with a mixture of acetonitril/0.1N ammonium-chloride (8/2, v/v). The average recoveries of acetamiprid and 6-chlornicotinic acid from sweet cherry samples were in the range of 95-101% and 73-83%, respectively, with the associated relative standard deviations (RSDs) lt 5%. Expanded measurement uncertainties for the analyzed compounds were 2.7 and 3.01%. The limit of quantification (LOQ) was 10 μg/kg and 30 μg/kg for acetamiprid and 6-chloronicotinic acid, respectively. Thus, the developed HPLC/DAD method can be considered a useful tool for sensitive and rapid determination of acetamiprid and 6-chloronicotinic acid. Hence, the method may find further application in the analysis of real sweet cherry samples contaminated with these insecticides at a ppb level., U radu je predstavljena jednostavna metoda za određivanje acetamiprida i njegovog metabolita, 6-hlornikotinske kiseline, u uzorcima trešanja. Metoda je bazirana na primeni reverzno-faznog razdvajanja na C18 koloni primenom gradijentnog eluiranja. Određivanje i kvantifikacija analita je vršena tečnom hromatografijom (HPLC) sa DAD detektorom, pri čemu je korišćena talasna dužina od 230 nm. Tačnost metode je ocenjena procenom merne nesigurnosti. Ekstrakcija acetamiprida i 6-hlornikotinske kiseline iz uzoraka trešanja je vršena smešom acetonitril/amonijum-hlorid (0,1N) u odnosu 80:20 (v/v). Sva merenja su vršena u tri ponavljanja, pri čemu su dobijeni prinosi određivanja acetamiprida i 6-hlornikotinske kiseline u rasponima 95-101% i 73-83%, respektivno. Relativne standardne devijacije (RSD) merenja su u svim slučajevima bile ispod 5%. Limiti kvantifikacije za acetamiprid i 6-HNK iznosili su 10 i 30 μg/kg, respektivno. Kombinovana merna nesigurnost rezultata analize acetamiprida i njegovog metabolita procenjena je na 1,35, odnosno 1,50%, a proširena na 2,7 i 3,01%, upotrebom faktora pokrivanja (k=2) koji odgovara nivou poverenja od 95%, za normalnu raspodelu. Nakon validacije i procene merne neizvesnosti dobijeni rezultati pokazuju da se razvijena HPLC/DAD metoda može primeniti za određivanje sadržaja acetamiprida i 6-hlornikotinske kiseline u uzorcima trešanja i relevantnim matriksima kontaminiranim ovim jedinjenjima.", publisher = "Institut za pesticide i zaštitu životne sredine, Beograd i Društvo za zaštitu bilja Srbije, Beograd", journal = "Pesticidi i fitomedicina", title = "Application of liquid chromatography with diode-array detector for determination of acetamiprid and 6-chloronicotinic acid residues in sweet cherry samples, Primena tečne hromatografije sa DAD detektorom za određivanje ostataka acetamiprida i 6-hlornikotinske kiseline u uzorcima trešanja", pages = "329-321", number = "4", volume = "27", doi = "10.2298/PIF1204321L" }
Lazić, S., Šunjka, D. B., Grahovac, N., Guzsvány, V., Bagi, F.,& Budakov, D.. (2012). Application of liquid chromatography with diode-array detector for determination of acetamiprid and 6-chloronicotinic acid residues in sweet cherry samples. in Pesticidi i fitomedicina Institut za pesticide i zaštitu životne sredine, Beograd i Društvo za zaštitu bilja Srbije, Beograd., 27(4), 321-329. https://doi.org/10.2298/PIF1204321L
Lazić S, Šunjka DB, Grahovac N, Guzsvány V, Bagi F, Budakov D. Application of liquid chromatography with diode-array detector for determination of acetamiprid and 6-chloronicotinic acid residues in sweet cherry samples. in Pesticidi i fitomedicina. 2012;27(4):321-329. doi:10.2298/PIF1204321L .
Lazić, Sanja, Šunjka, Dragana B., Grahovac, Nada, Guzsvány, Valéria, Bagi, Ferenc, Budakov, Dragana, "Application of liquid chromatography with diode-array detector for determination of acetamiprid and 6-chloronicotinic acid residues in sweet cherry samples" in Pesticidi i fitomedicina, 27, no. 4 (2012):321-329, https://doi.org/10.2298/PIF1204321L . .