Simultaneous determination of pesticides and 5-hydroxymethylfurfural in honey by the modified QuEChERS method and liquid chromatography coupled to tandem mass spectrometry

Abstract

Nowadays, bee products are being produced in an environment polluted by different sources of contamination, such as pesticides, which can be transported by honey bees to the hive and incorporated into honey. In addition, the increasing consumption of honey has demanded efficient quality control for this product. In this study, the determination of the pesticides fipronil, imidacloprid, thiamethoxam, dimethoate, carbendazin, tebuconazole, amitraz, τ-fluvalinate and 5-hydroxymethylfurfural (HMF) which are used as indicators of honey quality, was carried out simultaneously. For the sample preparation, the optimized QuEChERS method was used and the determinations were done by LC-APCI-MS/MS. The LOQs of the method ranged between 0.005 and 1.0 mg kg(-1). For the recovery calculations and method evaluation a working curve was drawn. All the analytical curves showed r values higher than 0.99. The recoveries ranged between 70% and 112%, with RSD lower than 20% for all compounds. The matrix effect was evaluated, and most of the compounds showed signal enrichment. The applicability of the method for honey from different flowers was verified, and the method showed robustness and recoveries in the range 70-120% established for all compounds in samples belonging to different blossoms. HMF was detected in all samples, with concentrations ranging between 4.6 and 51.7 mg kg(-1); it was below the maximum concentration allowed by the legislation.

Determination and surveillance of nine acaricides and one metabolite in honey by liquid chromatography-tandem mass spectrometry

“…However, amitraz is the one of the most difficult compounds to analyse because of its instability; moreover, it is easily degraded to metabolites such as 2,4-dimethylaniline (DMA), 2,4-dimethylformamidine (DMF) and N-2,4-dimethylphenyl-N-methylformamidine (DMPF) (Bernal et al 1997;Pierpoint et al 1997;Hepperle et al 2015). Therefore, amitraz extraction procedures should be carefully performed under basic conditions (Xu et al 2009;Tomasini et al 2012). Under restrictions in Japan, the MRL of amitraz is set as the sum of amitraz itself and 1.81 times the amount of DMPF (The Japan Food Chemical Research Foundation.…”

“…Thus far, some methodologies for analysing residual pesticides in honey have been developed (Debayle et al 2008;Blasco et al 2011;Tomasini et al 2012); however, these previous methods require expensive internal standards or involve quantification via matrix-matched *Corresponding author. Email: Takayuki_1_Nakajima@member.metro.tokyo.jp Food Additives & Contaminants: Part A, 2015 http://dx.doi.org/10.…”

One-Step QuEChERS-Based Approach to Extraction and Cleanup in Multiresidue Analysis of Sulfonylurea Herbicides in Cereals by Liquid Chromatography–Tandem Mass Spectrometry

“…One modification can be the choice of dispersive sorbent type(s), which depends on the analyte's properties and on the nature of co-extracts from the matrix. Primary and secondary amine (PSA), graphitized carbon black (GCB), or their combinations are commonly used sorbents (Lehotay et al 2010;Mantzos et al 2013;Tomasini et al 2012;Walorczyk et al 2015a). PSA retains many polar compounds, including sugars, organic acids, and fatty acids, and GCB removes pigments but adsorbs compounds with planar functionality (Walorczyk et al 2015b).…”

Reduction of matrix effects through a simplified QuEChERS method and using small injection volumes in a LC-MS/MS system for the determination of 28 pesticides in fruits and vegetables

“…[1][2][3] Matrix effects (MEs) can be classied into two categories: suppress the response of the analyte and enhance the response. 10 Moreover, several approaches to decrease MEs and improve recoveries have also been described, including: (1) several modied QuEChERS sample preparation methods; [11][12][13][14][15][16][17][18][19][20] (2) the internal standard method; 21 (3) dilution of matrix extraction; 4,8 (4) the microow approach 22 and (5) postcolumn infusion. [4][5][6] Once matrix components coeluted with the analyte, competition may occur between the matrix and analyte during the electrospray process.…”