Abstract
Background: Oxalic acid constitutes beekeepers′ leading choice for the battle of the parasitic mite Varroa destructor considering its efficacy, low cost, and easy application. Nevertheless, its broad use and reported synergistic effects prompted us to explore analytical methodologies for its determination in honeybees, especially after death incidents. Methods: The extraction of oxalic acid from bees was conducted by applying a simplified water extraction protocol. Oxalic acid′s content in honeybees was investigated through a novel zwiterionic hydrophilic interaction liquid chromatographic coupled to photo diode array (ZIC-HILIC-PDA) method and paralleled to gas/liquid chromatographic mass spectrometric methods. Results: The analytical method was validated, exhibiting a sufficient limit of quantification (LOQ) of 1.46 μg/g bee bw and precision and accuracy within the acceptable statistical limits as expressed by the relative standard deviation (RSD%) obtained from repeatability-reproducibility and recovery studies <12.5%. The application of the analytical method to 45 real honeybee samples demonstrated a fluctuation of oxalic acid’s concentrations from 1.6 to 1202.4 μg/g bee bw, verifying its frequent use in apiculture, exemplified by an overall 19% of positive samples. Conclusions: ZIC-HILIC-PDA proves a pivotal and alternative method to mass spectrometry tools in the determination of oxalic acid and other organic acids in honeybees and pertinent commodities.
Highlights
Oxalic acid (OA) is a simple non-aromatic organic acid naturally occurring in several food commodities and possessing a plethora of applications
It is among beekeepers0 top choices for the battle of the parasitic mite Varroa destructor considering its efficacy [1], low cost, and easy application in the beehive environment [2]
The exploitation of the photo diode array (PDA) in routine chemical analysis still constitutes an essential tool that can meet both sensitivity and selectivity requirements of modern chemical analysis, even for demanding matrices [19]. The latter was verified in this work, where PDA managed to detect OA with fit for purpose limit of detection (LOD) and limit of quantification (LOQ) with a retention time of 8.5 min
Summary
Oxalic acid (OA) is a simple non-aromatic organic acid naturally occurring in several food commodities (including honey) and possessing a plethora of applications. It is among beekeepers0 top choices for the battle of the parasitic mite Varroa destructor considering its efficacy [1], low cost, and easy application in the beehive environment [2]. Oxalic acid constitutes beekeepers0 leading choice for the battle of the parasitic mite Varroa destructor considering its efficacy, low cost, and easy application. Its broad use and reported synergistic effects prompted us to explore analytical methodologies for its determination in honeybees, especially after death incidents. The application of the analytical method to 45 real honeybee samples demonstrated a fluctuation of oxalic acid’s concentrations from 1.6 to
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