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
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Author
Lazic, Sanja
Sunjka, Dragana
Grahovac, Nada
Guzsvany, Valeria
Bagi, Ferenc
Budakov, Dragana
Keywords
Acetamiprid6-chloronicotinic acid
HPLC/DAD
Sweet cherry
Pesticide residues
6-hlornikotinska kiselina
trešnje
ostaci pesticida
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Show full item recordAbstract
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) <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.