Determination of acaricides in honeys from different botanical origins by gas chromatography-mass spectrometry

Development and Validation of a Gas Chromatography-Mass Spectrometry Method for Determining Acaricides in Bee Pollen

“…It is a well-known fact that the origin of bee pollen (geographical and botanical) is a main characteristic that significantly influences the analytical determination and chromatographic profile; even bee pollen of the same botanical origin can exhibit differences in their composition [ 22 ]. For these reasons, we decided to start by testing bee pollen samples in SCAN and SIM (Selected Ion Monitoring) mode (data not shown) ( n = 8; S1–S8) of different geographical origins purchased in local supermarkets, and using a similar procedure to that employed for determining acaricides in light honeys [ 19 ]. The SCAN mode provided a global visualization of the compounds present in the matrix.…”

“…The current trend in sample treatment prioritizes the use of solvents that are as least toxic as possible, in addition to being environmentally friendly [ 28 ], such as ethyl acetate and cyclohexane, which were evaluated in the presented study. Moreover, a combination of these solvents has been previously employed in the sample treatment of beehive products when determining pesticides [ 12 , 19 , 29 ]. Therefore, we decided to check the suitability of five different solvent mixtures that were chosen according to the related literature and previous experiments (see Supplementary Materials, Table S1 ).…”

“…The method validation was based on current legislation for pesticides residues analysis in food [ 21 ] and recent publications of our group [ 12 , 19 ]. Validation was performed with blank bee pollen, standards in the solvent, and standards in matrix extracts obtained according to the selected sample treatment.…”

“…However, they all focused mainly on a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method or on solid-phase extraction (SPE)-based sample treatments and the use of chromatography with mass spectrometry (MS) detectors [ 8 , 10 , 17 , 18 ]. It should be mentioned that gas chromatography (GC) has been predominantly selected for determining acaricides in bee pollen and other matrices due to the overall physicochemical characteristics of the acaricides [ 19 ]. However, some of these, such as coumaphos and chlorpyrifos, have also been determined by means of high-performance liquid chromatography (HPLC) [ 18 ].…”

“…Thus, the main goal of this paper is to propose an alternative method for the simultaneous determination of seven of the most frequently detected acaricides in bee products around the world (atrazine, chlorpyrifos, chlorfenvinphos, α-endosulfan, bromopropylate, coumaphos, and τ-fluvalinate; see Table 1 ) in bee pollen samples through the use of GC-MS. We have adapted the GC-MS conditions from a recent study of our group [ 19 ], as we wanted to focus our efforts in developing an efficient, simple, economic, and fast sample treatment. In addition, we have performed the method optimization with the aim of obtaining the best extraction efficiency (recovery values), minimizing the matrix effect as much as possible, and fulfilling the principles of green analytical chemistry (reducing the number and amount of reagents, reducing time, and costs) [ 20 ].…”