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

  • Sanja D Lazić Univerzitet u Novom Sadu Poljoprivredni fakultet Departman za fitomedicinu i zaštitu životne sredine
  • Dragana B Šunjka University of Novi Sad Faculty of Agriculture
  • Nada L Grahovac Institute for Crops and Vegetables, Novi Sad
  • Valéria J Guzsvány University of Novi Sad Faculty of Science
  • Ferenc F Bagi University of Novi Sad Faculty of Agriculture
  • Dragana B Budakov University of Novi Sad Faculty of Agriculture
Ključne reči: Pesticide residues||, ||Ostaci pesticida, Sweet cherry||, ||trešnje, HPLC/DAD||, ||HPLC/DAD, 6-chloronicotinic acid||, ||6-hlornikotinska kiselina, Acetamiprid||, ||Acetamiprid,

Sažetak


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-hlor nikotinske 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.

Biografije autora

Sanja D Lazić, Univerzitet u Novom Sadu Poljoprivredni fakultet Departman za fitomedicinu i zaštitu životne sredine

Department for Environmental and Plant protection

PhD

Dragana B Šunjka, University of Novi Sad Faculty of Agriculture

Department for Environmental and Plant protection

MSc

Nada L Grahovac, Institute for Crops and Vegetables, Novi Sad
MSc
Valéria J Guzsvány, University of Novi Sad Faculty of Science

Department of Chemistry, Biochemistry and Environmental Protection

PhD

Ferenc F Bagi, University of Novi Sad Faculty of Agriculture

Department for Environmental and Plant protection

PhD

Dragana B Budakov, University of Novi Sad Faculty of Agriculture

Department for Environmental and Plant protection

MSc

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