Dataset Information

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

ABSTRACT: Pesticides can be found in beehives for several reasons, including contamination from surrounding crops or for their use by beekeepers, which poses a risk to bee ecosystems and consumers. Therefore, efficient and sensitive methods are needed for determining pesticide residues in bee products. In this study, a new analytical method has been developed and validated to determine seven acaricides (atrazine, chlorpyrifos, chlorfenvinphos, α-endosulfan, bromopropylate, coumaphos, and τ-fluvalinate) in bee pollen using gas chromatography coupled to mass spectrometry. After an optimization study, the best sample treatment was obtained when using a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method employing an ethyl acetate and cyclohexane as the extractant mixture, and a mixture of salts for the clean-up step. A chromatographic analysis (<21 min) was performed in an Agilent DB-5MS column, and it was operated under programmed temperature conditions. The method was fully validated in terms of selectivity, limits of detection (0.2-3.1 µg kg^-1) and quantification (0.6-9.7 µg kg^-1), linearity, matrix effect (<20% in all cases), trueness (recoveries between 80% and 108%), and precision. Finally, the proposed method was applied to analyze commercial bee pollen samples, and some of the target pesticides (chlorfenvinphos, α-endosulfan, coumaphos, and τ-fluvalinate) were detected.

SUBMITTER: Fuente-Ballesteros A

PROVIDER: S-EPMC10056623 | biostudies-literature | 2023 Mar

REPOSITORIES: biostudies-literature

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

Fuente-Ballesteros Adrián A Augé Camille C Bernal José J Ares Ana M AM

Molecules (Basel, Switzerland) 20230309 6

Pesticides can be found in beehives for several reasons, including contamination from surrounding crops or for their use by beekeepers, which poses a risk to bee ecosystems and consumers. Therefore, efficient and sensitive methods are needed for determining pesticide residues in bee products. In this study, a new analytical method has been developed and validated to determine seven acaricides (atrazine, chlorpyrifos, chlorfenvinphos, α-endosulfan, bromopropylate, coumaphos, and τ-fluvalinate) in ...[more]

PMID: 36985469

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Project description:The research into new pharmaceutical substances based on essential oils, individual biologically active phytochemicals, and plant extracts is a priority in field of pharmaceutical sciences. A novel multicomponent substance based on Melaleuca alternifolia (M. alternifolia) leaf oil (TTO), 1,8-cineole (eucalyptol), and (-)-α-bisabolol with potent synergetic antimicrobial activity was investigated and suggested for the treatment of seborrheic dermatitis (SD) and dandruff. The objective of this research was to establish and validate a specific, accurate, and precise gas chromatography-mass spectrometry (GC-MS) method for further quantitative and qualitative analysis in order to ensure quality control. The main parameters of validation were suitability, specificity, linearity, accuracy, and intermediate precision according to the European Pharmacopoeia (XI edition), Russian Pharmacopoeia (XIV edition), and some parameters of ICH requirements. The peaks of fifteen chemical phytoconstituents were identified in the test sample solution with the prevalence of (-)-α-bisabolol (27.67%), 1,8-cineole (25.63%), and terpinen-4-ol (16.98%). These phytochemicals in the novel substance were chosen for standardization and validation of the GC-MS method. The chosen chromatographic conditions were confirmed for testing of the plant-based substance in a suitability test. It was established that the GC-MS method provides a significant separation, symmetry of peaks and resolution between phytochemicals. The calibration curves of each phytochemical had good linearity (R2 > 0.999) in five concentrations. In the same concertation range, the accuracy of terpinen-4-ol, 1,8-cineol, and (-)-α-bisabolol determination using the method of additives was 98.3-101.60%; the relative standard deviation (RSD) ranged from 0.89% to 1.51% and corresponded to requirements. The intraday and interday precision was ≤2.56%. Thus, the GC-MS method was validated to be specific, sensitive, linear, accurate, and precise. This GC-MS method could be recommended as a routine analytic technique for multicomponent plant-based substances-enriched terpenes.

Dataset Information

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

Publications

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

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