Gas chromatography–mass spectrometry determination of deltamethrin in food

I.M. Fitsev^*, E.R. Rakhmetova^**, A.G. Mukhammetshina^***, K.E. Burkin^****, O.V. Shlyamina^*****

Federal Center for Toxicological, Radiation, and Biological Safety, Kazan, 420075 Russia

E-mail: ^*fitzev@mail.ru, ^**elvira_rakhmetova@mail.ru, ^***aika.muha@yandex.ru, ^****konstantinburkin@yandex.ru, ^*****shlyamina@mail.ru

Received June 23, 2021

ORIGINAL ARTICLE

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DOI: 10.26907/2542-064X.2021.4.569-580

For citation: Fitsev I.M., Rakhmetova E.R., Mukhammetshina A.G., Burkin K.E., Shlya­mina O.V. Gas chromatography–mass spectrometry determination of deltamethrin in food. Uchenye Zapiski Kazanskogo Universiteta. Seriya Estestvennye Nauki, 2021, vol. 163, no. 4, pp. 569–580. doi: 10.26907/2542-064X.2021.4.569-580. (In Russian)

Abstract

The article presents the results of the determination of the synthetic pyrethroid deltamethrin in raw food and various food products by gas chromatography with mass spectrometric detection (GC–MS). The stage of GC–MS determination is preceded by sample preparation using the QuEChERS method.

The developed method for quantitative determination of deltamethrin by GC–MS with electron ionization (EI, 70 eV) in food products using QuEChERS is characterized by a detection limit of 0.9 µg/kg deltamethrin and a standard deviation not exceeding 5%.

The GC–MS quantitative determination of ultra-low deltamethrin content in food was performed in selected ion mode (SIM/SIR mode). The selected ions were m/z 253 (main ion) and m/z 208, 181 (confirming ions), respectively.

Keywords: toxicological control of food, organic pollutants, deltamethrin, gas chromatography–mass spectrometry, QuEChERS

Acknowledgments. We are grateful to the Federal Center for Toxicological, Radiation, and Biological Safety for providing us with the analytical equipment used in this study.

Figure Captions

Fig. 1. Scheme of sample preparation using the QuEChERS method for determining deltamethrin by GC–MS.

Fig. 2. Influence of the sorbents Florisil, PSA, and C18 on the degree of extraction of deltamethrin from food samples: a) fruits and vegetables; b) fish; c) meat.

Fig. 3. EI mass spectrum (70 eV) of deltamethrin and main directions of dissociative ionization of its molecule.

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