Development and Validation of a Gas Chromatography-Mass Spectrometry Method for Determining Acaricides in Bee Pollen
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 thi...
| Main Authors: | , , , |
|---|---|
| Format: | Article |
| Language: | English |
| Published: |
MDPI AG
2023-03-01
|
| Series: | Molecules |
| Subjects: | |
| Online Access: | https://www.mdpi.com/1420-3049/28/6/2497 |
| _version_ | 1797609897138847744 |
|---|---|
| author | Adrián Fuente-Ballesteros Camille Augé José Bernal Ana M. Ares |
| author_facet | Adrián Fuente-Ballesteros Camille Augé José Bernal Ana M. Ares |
| author_sort | Adrián Fuente-Ballesteros |
| collection | DOAJ |
| description | 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<sup>−1</sup>) and quantification (0.6–9.7 µg kg<sup>−1</sup>), 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. |
| first_indexed | 2024-03-11T06:08:00Z |
| format | Article |
| id | doaj.art-127f9e06a93c41dfb337cb360906aeb9 |
| institution | Directory Open Access Journal |
| issn | 1420-3049 |
| language | English |
| last_indexed | 2024-03-11T06:08:00Z |
| publishDate | 2023-03-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj.art-127f9e06a93c41dfb337cb360906aeb92023-11-17T12:51:10ZengMDPI AGMolecules1420-30492023-03-01286249710.3390/molecules28062497Development and Validation of a Gas Chromatography-Mass Spectrometry Method for Determining Acaricides in Bee PollenAdrián Fuente-Ballesteros0Camille Augé1José Bernal2Ana M. Ares3Analytical Chemistry Group (TESEA), I.U. CINQUIMA, Faculty of Sciences, University of Valladolid, 47011 Valladolid, SpainSIGMA Clermont, Clermont-Ferrand Campus, 63178 Aubiere, FranceAnalytical Chemistry Group (TESEA), I.U. CINQUIMA, Faculty of Sciences, University of Valladolid, 47011 Valladolid, SpainAnalytical Chemistry Group (TESEA), I.U. CINQUIMA, Faculty of Sciences, University of Valladolid, 47011 Valladolid, SpainPesticides 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<sup>−1</sup>) and quantification (0.6–9.7 µg kg<sup>−1</sup>), 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.https://www.mdpi.com/1420-3049/28/6/2497acaricidesbee pollengas chromatography-mass spectrometrymethod validationQuEChERSsample treatment |
| spellingShingle | Adrián Fuente-Ballesteros Camille Augé José Bernal Ana M. Ares Development and Validation of a Gas Chromatography-Mass Spectrometry Method for Determining Acaricides in Bee Pollen Molecules acaricides bee pollen gas chromatography-mass spectrometry method validation QuEChERS sample treatment |
| title | Development and Validation of a Gas Chromatography-Mass Spectrometry Method for Determining Acaricides in Bee Pollen |
| title_full | Development and Validation of a Gas Chromatography-Mass Spectrometry Method for Determining Acaricides in Bee Pollen |
| title_fullStr | Development and Validation of a Gas Chromatography-Mass Spectrometry Method for Determining Acaricides in Bee Pollen |
| title_full_unstemmed | Development and Validation of a Gas Chromatography-Mass Spectrometry Method for Determining Acaricides in Bee Pollen |
| title_short | Development and Validation of a Gas Chromatography-Mass Spectrometry Method for Determining Acaricides in Bee Pollen |
| title_sort | development and validation of a gas chromatography mass spectrometry method for determining acaricides in bee pollen |
| topic | acaricides bee pollen gas chromatography-mass spectrometry method validation QuEChERS sample treatment |
| url | https://www.mdpi.com/1420-3049/28/6/2497 |
| work_keys_str_mv | AT adrianfuenteballesteros developmentandvalidationofagaschromatographymassspectrometrymethodfordeterminingacaricidesinbeepollen AT camilleauge developmentandvalidationofagaschromatographymassspectrometrymethodfordeterminingacaricidesinbeepollen AT josebernal developmentandvalidationofagaschromatographymassspectrometrymethodfordeterminingacaricidesinbeepollen AT anamares developmentandvalidationofagaschromatographymassspectrometrymethodfordeterminingacaricidesinbeepollen |