Abstract
There is an increasing interest on neonicotinoid residues determination in honey samples because they are banned by European Union. Their determination is based on liquid chromatography analytical methods and, therefore, the aim of this study was to develop the analytical method for quantifying these compounds using different sample preparation techniques. The sample preparation was conducted by two different techniques and the new HPLC-DAD method was developed and validated assuring reliable accuracy (R, 70-120 %), repeatability (RSD, < 20 %) and within-laboratory reproducibility (RSD, <20 %). Also, low limits of detection and quantification (LOD, 2.5-5.0 μg kg-1; LOQ, 7.5-10.0 μg kg-1) for the mentioned method were achieved. To address the importance of honey safety control more than 100 samples from Vojvodina region were analyzed showing residues of neonicotinoids. The HPLC-MS/MS method was used to confirm the presence of neonicotinoids quantified using validated HPLC-DAD method.
Highlights
The most widely used class of the insecticides in last 20 years are neonicotinoids, which act as a receptor agonists of nicotinic acetylcholine (Decourtye and Devillers, 2010; Tomizawa and Casida, 2005)
The mobile phase consisted of two eluents, ACN (A) and 100.0 μg kg-1 concentration levels calculated with MMC
Limits of detection and limits of quantification are the indicators of method sensitivity in residue analysis, and with the achieved limit of detection (LOD) of 2.5–5.0 μg kg-1 and limit of quantification (LOQ) of 7.5–10.0 μg kg-1 we can assume that this method is applicable for the neonicotinoid residue analysis
Summary
The most widely used class of the insecticides in last 20 years are neonicotinoids, which act as a receptor agonists of nicotinic acetylcholine (Decourtye and Devillers, 2010; Tomizawa and Casida, 2005). The residues of neonicotinoids may be found in honey, pollen and other bee product (Kasiotis et al, 2014; Tanner and Czerwenka, 2011). Due to their evidenced negative impact, the European Commission issued two-year ban for the use of thiamethoxam, imidacloprid and clothianidin in crops attractive to bees (Commission, 2013; EFSA, 2013). The main goal of this research was development of rapid, sensitive, optimized and reliable liquid chromatography method with DAD detector in alliance with chosen extraction techniques for determination of dinotefuran, thiamethoxam, clothianidin, acetamiprid, imidacloprid, nitenpyram, and thiacloprid in honey. The proposed method was validated and applied to around hundred honey samples for the presence of the neonicotinoids (Jovanov, 2014)
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