Dissipation rate of acetamiprid in sweet cherries
Razgradnja acetamiprida u plodovima trešanja
Pregled/ Otvaranje
Autor
Lazic, Sanja
Sunjka, Dragana
Panic, Srdjan
Indjic, Dusanka
Grahovac, Nada
Guzsvany, Valeria
Jovanov, Pavle
Ključne reči
AcetamipridSweet cherries
Dissipation
Residues
acetamprid
trešnje
razgradnja
ostaci
Metadata
Prikaz svih podataka o dokumentuApstrakt
Degradation of acetamiprid in sweet cherry samples was evaluated at several intervals
from the product application until the end of the pre-harvest interval. An orchard
of sweet cherries located at Stepanovićevo village near Novi Sad was used in this study.
Acetamiprid was applied according to the manufacturer’s recommendation for protecting
sweet cherries from their most important pests. Sweet cherry fruit samples were collected
at eight intervals: immediately after acetamiprid application and 2, 4, 6, 8, 10, 12
and 14 days after application. The extraction of acetamiprid from sweet cherry samples
was performed using a QuEChERS-based method. Determination was carried out using
an HPLC-UV diode array detection system (Agilent 1100, United States) with an Agilent
Zorbax Eclipse C18 column (50 mm × 4.6 mm internal diameter, 1.8 μm particle size).
The method was subjected to a thorough validation procedure. The recovery data were
obtained by spiking blank sweet cherry samples at three concentration levels (0.1-0.3 mg/
kg), yielding 85.4% average recovery. Precision values expressed as relative standard deviation
(RSD) were below 1.61% for the intraday precision. Acetamiprid showed linear calibrations
from 0.05 to 2.5 μg/ml with correlation coefficient (R2) of 0.995%. The limit of
detection and limit of quantification were found to be 5 μg/kg and 14 μg/kg, respectively.
The validated method was applied in the analysis of acetamiprid in sweet cherry samples.
During the study period, the concentration of acetamiprid decreased from 0.529
mg/kg to 0.111 mg/kg. The content of acetamiprid in sweet cherry samples at the end
of the pre-harvest interval was below the maximum permissible level specified by the
Serbian and EU MRLs. U cilju praćenja razgradnje acetamiprida u plodovima trešanja u periodu od primene
preparata do isteka karence, izvršen je tretman preparatom na bazi ove aktivne materije
u preporučenoj dozi. Ogled je postavljen u zasadu srednje kasne sorte trešnje na lokalitetu
Stepanovićevo u okolini Novog Sada. Plodovi su uzorkovani osam puta – odmah nakon
primene preparata, 2, 4, 6, 8, 10, 12 i 14 dana. Ekstrakcija acetamiprida iz trešanja izvedena
je QuEChERS metodom. Za određivanje acetamiprida korišćena je tečna hromatografija sa
DAD detektorom (Agilent 1100, United States) i Agilent Zorbax Eclipse C18 kolonom (unutrašnji
prečnik 50 mm x 4.6 mm, veličina čestica 1.8 μm). Kao mobilna faza upotrebljeni su
acetonitril i 1.5% rastvor CH3COOH (30/70), sa protokom 1 ml/min, temperaturom kolone
25 oC i injektovanom zapreminom 2,5 μl, dok je kao odgovarajuća talasna dužina usvojena
vrednost od 254 nm. Validacija metode je u potpunosti sprovedena u skladu sa zahtevima
standarda SANCO/12495/2011 (EU Commission Health and Consumer Protection Directorate-
General, 2011). Prosečna vrednost prinosa ekstrakcije acetamiprida iz trešanja proverena
na tri nivoa obogaćenja (0.1-0.3 mg/kg) iznosila je 85.4%. Preciznost merenja razmotrena
proverom ponovljivosti određivanja acetamiprida izražena je relativnom standardnom
devijacijom (RSD) sa vrednošću manjom od 1.61%. U opsegu masenih koncentracija acetamiprida
od 0,05 do 2,5 μg/ml postignuta je dobra linearnost odziva detektora sa koeficijentom
varijacije od 0,995%. Limit detekcije i kvantifikacije za određivanje acetamiprida
u trešnjama prikazanom metodom iznose 5 μg/kg i 14 μg/kg. Tokom ispitivanog perioda
koncentracija acetamiprida u trešnjama se smanjivala od 0,592 mg/kg neposredno nakon
primene insekticida do 0,111 mg/kg po isteku karence od 14 dana. Analizom je utvrđeno
da je sadržaj acetamiprida u uzorcima plodova trešnje nakon isteka perioda karence ispod
maksimalno dozvoljene količine za ovu aktivnu materiju propisane Pravilnikom Republike
Srbije (0,2 mg/kg) i Evropske Unije (1,5 mg/kg).