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Primena tečne hromatografije sa DAD detektorom za određivanje ostataka acetamiprida i 6-hlornikotinske kiseline u uzorcima trešanja

dc.contributor.authorLazic, Sanja
dc.contributor.authorSunjka, Dragana
dc.contributor.authorGrahovac, Nada
dc.contributor.authorGuzsvany, Valeria
dc.contributor.authorBagi, Ferenc
dc.contributor.authorBudakov, Dragana
dc.date.accessioned2015-11-08T15:07:28Z
dc.date.available2015-11-08T15:07:28Z
dc.identifier.urihttp://arhiva.nara.ac.rs/handle/123456789/1459
dc.description.abstractA 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) <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.en
dc.description.abstractU 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.sr
dc.subjectAcetamipridsr
dc.subject6-chloronicotinic aciden
dc.subjectHPLC/DADen
dc.subjectSweet cherryen
dc.subjectPesticide residuesen
dc.subject6-hlornikotinska kiselinasr
dc.subjecttrešnjesr
dc.subjectostaci pesticidasr
dc.titleApplication of Liquid Chromatography with Diode-Array Detector for Determination of Acetamiprid and 6-chloronicotinic Acid Residues in Sweet Cherry Samplesen
dc.title.alternativePrimena tečne hromatografije sa DAD detektorom za određivanje ostataka acetamiprida i 6-hlornikotinske kiseline u uzorcima trešanjasr


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