Naslov
Analysis and validation of multiresidue pesticides in honey - followed by GC-MS/MS

Autori
Jurak Gordana, Bošnir Jasna, Krivohlavek Adela, Bešlić P. Iva

Vrsta, podvrsta i kategorija rada
Sažeci sa skupova, sažetak, stručni

Skup
14th European Pesticide Residues Workshop

Mjesto i datum
Bologna, Italija, 19.09.2022. - 23.09.2022

Vrsta sudjelovanja
Poster

Vrsta recenzije
Međunarodna recenzija

Ključne riječi
honey, pesticides, project, GC-MS/MS, LC-MS/MS

Sažetak
Honey is produced by bees (Apis mellifera) from the nectar of honey plants or plant secretions. The absorbent surface (waxes) and high concentration of sugars with low water content make honey a suitable matrix for pesticide deposition. For the purposes of this study, samples were collected from domestic (Croatia) honey producers in glass jars with screw caps. Validation was performed following document SANTE/2021/11312.A total of 50 samples were analyzed for 243 pesticides residues. Samples of honey were prepared using the modified „Quechers” method EN 15662:2018. Before extraction, the samples were well homogenized and 5 g of samples were weighed. Adding 5 ml water. The internal TPP standard, 10 ml ACN, 4 mg MgSO4, 1 g NaCl, 1 g trisodium citrate dehydrate and 0.5 g disodium hydrogen sesquihydrate are added to the sample. The sample thus prepared is centrifuged for 5 min at 4500 rpm. An aliquot of 6 ml upper phase of ACN was taken further for the dSPE clean up. Pre- prepared tubes containing 150 mg primary, secondary amine (PSA), 150 mg C18 and 900 mg magnesium sulfate are used for removing co- extracted compounds from the matrix. After 5 min centrifugation at 4500 rpm samples were frozen at -20 C for four hours. One milliliter of prepared sample is transferred to a dark vial. Analysis was performed using Shimadzu TQ-8050NX GC-MS/MS and a computer equipped with LabSolution Insight software. The three ion transitions for MRM of each pesticide were determined. The method was validated in honey, including limits of quantification of LOQ as lowest spiking level of 0.01 mg/kg meeting acceptability criteria. Recovery was carried out in two spiking levels (0.01 and 0.02 mg/kg) meeting the criteria of 70- 120% recovery. Repeatability (RSD) with ≤ 20% for each tested spiking level was tested (Table 1). For sample quantification, a matrix matched standard of “blank” honey extract was prepared at concentrations that meet the limit of quantification (LOQ) of 0.01 mg/kg. From 50 samples, in 5 samples, residues of Coumaphos were detected and quantified in the range 0.019-0.34 mg/kg. In three samples the amount of Coumaphos exceeded MRL (0.1 mg/kg). In the honey matrix of 260 analyzed pesticides, 243 analytes meet the set validation criteria according to SANTE/2021/11312. From 50 analyzed honey samples collected in Croatia, 3 samples contain pesticide residue of Coumaphos above MRL, and they are assessed as non- compliant.

Izvorni jezik
Engleski

Znanstvena područja
Kemijsko inženjerstvo, Javno zdravstvo i zdravstvena zaštita

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