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Development and validation of the method for determination of amitraz in honey using high-performance liquid chromatography with mass spectrometric detection

https://doi.org/10.29235/1561-8331-2022-58-4-387-397

Abstract

Method for determination of the insecticide amitraz residual content in honey has been developed and validated. The method is selective, express and easy-to-perform. The technique is based on the extraction of amitraz from alkalized aqueous solutions of honey with n-hexane and quantitative determination by high-performance liquid chromatography with mass spectrometric detection. Validation was performed using three types of honey at three levels of amitraz application 6, 120 and 220 µg/kg. The limit of quantification was 0.9 µg/kg, the calibration curves were linear in the concentration range from 2.5 to 125.0 ng/mL (the corresponding analyte content in honey is from 5.0 to 250.0 µg/kg), relative values of the standard deviations of repeatability and within-laboratory reproducibility did not exceed 3.4 and 5.9 %, respectively, the bias values varied from –8.2 to 5.6 %, the expanded uncertainty estimates of the results ranged from 12 to 16 % (P = 0.95). Instrumental limit of quantification, overall efficiency of the process and robustness were also evaluated during the validation process.

About the Authors

A. G. Polonevich
Scientific Practical Center of Hygiene
Belarus

Polonevich Anna G. – Doctoral student at the Department of Analytical Chemistry; Leading Chemist.

14, Leningradskaya str., 220030; 8, Akademicheskaya str., 220012, Minsk



S. M. Leschev
Belarusian State University
Belarus

Leschev Sergey M. – Ph. D. (Chemistry), Professor.

14, Leningradskaya str., 220030



V. A. Bulhakava
Scientific Practical Center of Hygiene
Belarus

Bulhakava Volha A. – Chemist.

8, Akademicheskaya str., 220012, Minsk



L. L. Belyshava
Scientific Practical Center of Hygiene
Belarus

Belysheva Liudmila L. – Head of the Laboratory.

8, Akademicheskaya Str., 220012, Minsk



References

1. Gupta R. C. (ed.). Amitraz. Veterinary Toxicology. Basic and Clinical Principles. 3d ed. Academic Press, 2018, pp. 525–531. https://doi.org/10.1016/B978-0-12-811410-0.00041-6

2. Weijia Zheng, Jin-A. Park, A. M. Abd El-Aty, Seong-Kwan Kim, Sang-Hyun Cho, Jeong-min Choi, Hee Yi, Soo-Min Cho, Amer Ramadan, Ji Hoon Jeong, Jae-Han Shim, Ho-Chul Shin. Development and validation of modified QuEChERS method coupled with LC–MS/ MS for simultaneous determination of cymiazole, fipronil, coumaphos, fluvalinate, amitraz, and its metabolite in various types of honey and royal jelly. Journal of Chromatography B, vol. 1072, 2018, pp. 60–69. https://doi.org/10.1016/j.jchromb.2017.11.011

3. Council of the Eurasian Economic Commission. TR [Customs Union Technical Regulation] TS 021/2011. On the Safety of Food Products. Minsk, Energopress Publ., 2021. 144 p. (in Russian).

4. Julia Hepperle, Dorothea Mack, Irina Sigalov, Sigrid Schüler, Michelangelo Anastassiades. Analysis of “Amitraz (sum)” in pears with incurred residues – Comparison of the approach covering the individual metabolites via LC–MS/MS with the approach involving cleavage to 2,4-dimethylaniline. Food Chemistry, vol. 166, 2015, pp. 240–247, https://doi.org/10.1016/j.foodchem.2014.06.003

5. Yumi Ohba, Takayuki Nakajima, Maki Kanda, Hiroshi Hayashi, Youko Matsushima, Yukiko Nakagawa, Hiroshi Koike, Chieko Nagano, Kotaro Sekimura, Kenji Otsuka, Takeo Sasamoto, Tsuneo Hashimoto. Simultaneous determination of nine acaricides and two metabolites in comb honey by LC/MS/MS. Food Additives and Contaminants: Part A, 2018, vol. 35, iss. 12, pp. 2375–2386. https://doi.org/10.1080/19440049.2018.1539252

6. Tomasz Kiljanek, Alicja Niewiadowska, Stanisław Semeniuk, Marta Gaweł, Milena Borzęcka, Andrzej Posyniak. Multi-residue method for the determination of pesticides and pesticide metabolites in honeybees by liquid and gas chromatography coupled with tandem mass spectrometry–Honeybee poisoning incidents. Journal of Chromatography A, 2016, vol. 1435, pp. 100–114. https://doi.org/10.1016/j.chroma.2016.01.045

7. Charmaine M. van Eeden, Wilna Liebenberg, Jan L. du Preez & Melgardt M. de Villiers. Solvent and Surfactant Enhanced Solubilization, Stabilization, and Degradation of Amitraz. Journal of Environmental Science and Health, Part B, 2004, vol. 39, no. 1, pp. 33–51. https://doi.org/10.1081/PFC-120027437

8. Pablo R. Duchowicz, Alan Talevi, Luis E. Bruno-Blanch, Eduardo A. Castro. New QSPR study for the prediction of aqueous solubility of drug-like compounds. Bioorganic & Medicinal Chemistry, 2008, vol. 16, iss. 17, pp. 7944–7955. https://doi.org/10.1016/j.bmc.2008.07.067

9. Corta E., Bakkali A., Berrueta L. A., Gallo B., Vicente F. Kinetics and mechanism of amitraz hydrolysis in aqueous media by HPLC and GC-MS. Talanta, 1999, vol. 48, iss. 1, pp. 189–199. https://doi.org/10.1016/S0039-9140(98)00237-9

10. International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH), Q2 (R1): Validation of Analytical Procedures: Text and Methodology. Available at: https://database.ich.org/sites/default/files/Q2(R1)%20Guideline.pdf.

11. STB ISO 11095-2009. Linear calibration using reference materials. Minsk, Belarusian state Institute of Stan dardi zation and Certification, 2009. 31 p. (in Russian).

12. Calculation of Measurement Uncertainty in Environmental Laboratories. Nordtest Technical Report 537, 2017. Available at: http://nordtest.info/images/documents/nt-technical-reports/NT_TR_537_edition4_English_Handbook_for_calculation_of_measurement_uncertainty_in_environmental_laboratories.pdf

13. Analytical quality control and method validation procedures for pesticide residues analysis in food and feed SANTE/12682/2019. Available at: https://www.eurl-pesticides.eu/userfiles/file/EurlALL/AqcGuidance_SANTE_2019_12682.pdf

14. Treatment of an observed bias (information leaflet). Available at: https://www.eurachem.org/images/stories/leaflets/mu/bias_01/Eurachem_Bias_Leaflet_01_EN.pdf


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ISSN 1561-8331 (Print)
ISSN 2524-2342 (Online)