Determination of Carvacrol and Thymol in Honey by Using a Simple and Efficient Headspace-Gas Chromatography-Mass Spectro
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Determination of Carvacrol and Thymol in Honey by Using a Simple and Efficient Headspace-Gas Chromatography-Mass Spectrometry Method José Bernal 1 & María J. Nozal 1 & José L. Bernal 1 & Ana M. Ares 1 Received: 21 July 2020 / Accepted: 29 July 2020 # Springer Science+Business Media, LLC, part of Springer Nature 2020
Abstract A novel method has been proposed to determine residues of thymol and carvacrol in honey, by means of a headspace coupled to a gas chromatography-mass spectrometer. No sample treatment was required, since the samples were injected directly after selection of the optimal headspace operating conditions, in this case, an equilibration time of 7 min and temperatures of 150 °C, 170 °C, or 175 °C for the oven, loop, and transfer line, respectively. The chromatographic conditions were also optimized, with a ZB-WAX (60 m × 0.25 mm × 25 μm) column, the helium carrier gas at a flow rate of 1.1 mL/min, and a temperature program allowing baseline separation of both compounds in under 18 min. Thymol and carvacrol should be quantified in honey samples with matrix-matched standard calibration curves, although samples from rosemary and orange blossom, as well as those of multifloral and heather botanical origins, respectively, can be determined with the same calibration curves. Not only was the proposed method selective, but it was also accurate (relative standard deviation values under 6%) and sensitive (detection and quantification limits lower than 40 μg/kg). Several honey samples were analyzed, and thymol and carvacrol residues were found at low concentrations (quantification limit-97 μg/kg) in some cases. Keywords Carvacrol . Food analysis . Gas chromatography-mass spectrometry . Headspace . Honey . Thymol
Introduction Beekeeping, which is directly related with the production of some foods like honey, bee pollen royal jelly, and propolis, has been affected in the last few years by a drastic reduction in the number of honey bees (Apis mellifera) and the loss of numerous beehives, observed in many countries around the world (Neuman and Carreck 2010). This phenomenon, which is known as colony collapse disorder, has been extensively investigated, and the current hypothesis regarding a multi-causal etiology is generally accepted: the synergistic effect of pesticides, infectious diseases, climate changes, poor nutritional sources, and beekeeping practices may result in a substantial effect (Porrini et al. 2016). In particular, the Varroa destructor mite is considered to be one of the most destructive pests for the honey bee, perhaps even * Ana M. Ares [email protected]; http://tesea.uva.es/ 1
I. U. CINQUIMA, Analytical Chemistry Group, Faculty of Sciences, University of Valladolid, Paseo de Belén 5, 47011 Valladolid, Spain
leading to the death of entire colonies. Consequently, beekeepers have to decide on a treatment in order to keep their beehives in a healthy condition (Tonello et al. 2016). Synthetic acaricides have been used in the past, but their intensive use and their degradation products have gen
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