vestichИзвестия Национальной академии наук Беларуси. Серия химических наукProceedings of the National Academy of Sciences of Belarus, Chemical Series1561-83312524-2342The Republican Unitary Enterprise Publishing House "Belaruskaya Navuka"10.29235/1561-8331-2022-58-4-387-397vestich-763Research ArticleАНАЛИТИЧЕСКАЯ ХИМИЯANALYTICAL CHEMISTRYРазработка и валидация методики определения амитраза в меде высокоэффективной жидкостной хроматографией с масс-спектрометрическим детектированиемDevelopment and validation of the method for determination of amitraz in honey using high-performance liquid chromatography with mass spectrometric detectionПолоневичА. Г.PolonevichA. G.

Полоневич Анна Геннадьевна – соискатель кафедры аналитической химии; ведущий химик.

Ул. Ленинградская, 14, 220030, Минск; Ул. Академическая, 8, 220012, Минск

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

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

gannapalanevich@gmail.comЛещевС. М.LeschevS. M.

Лещев Сергей Михайлович – доктор химических наук, про фес сор

Ул. Ле нинградская, 14, 220030, Минск

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

14, Leningradskaya str., 220030

leschev.sergey54@gmail.comБулгаковаО. А.BulhakavaV. A.

Булгакова Ольга Анатольевна – химик.

Ул. Академическая, 8, 220012, Минск

Bulhakava Volha A. – Chemist.

8, Akademicheskaya str., 220012, Minsk

mjuse@rambler.ruБелышеваЛ. Л.BelyshavaL. L.

Белышева Людмила Леонидовна – заведующий лабораторией.

Ул. Академическая, 8, 220012, Минск

Belysheva Liudmila L. – Head of the Laboratory.

8, Akademicheskaya Str., 220012, Minsk

llbelysheva@gmail.comНаучно-практический центр гигиеныScientific Practical Center of HygieneБелорусский государственный университетBelarusian State University202229112022584387397Copyright © Полоневич А.Г., Лещев С.М., Булгакова О.А., Белышева Л.Л., 20222022Полоневич А.Г., Лещев С.М., Булгакова О.А., Белышева Л.Л.Polonevich A.G., Leschev S.M., Bulhakava V.A., Belyshava L.L.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://vestichem.belnauka.by/jour/article/view/763

Разработана и валидирована селективная, экспрессная, простая в исполнении методика опре деления остаточного содержания инсектицида амитраз в меде. Методика основана на экстрагировании амитраза из подщелаченного водного раствора меда н-гексаном и количественном определении методом высокоэффективной жидкостной хроматографии с масс-спектрометрическим детектированием. Валидацию проводили с использованием трех видов меда на трех уровнях внесения амитраза 6, 120 и 220 мкг/кг. Предел определения составил 0,9 мкг/кг, градуировочные графики линейны в диапазоне концентраций от 2,5 до 125,0 нг/мл (соответствующее содержание аналита в меде – от 5,0 до 250,0 мкг/кг), относительные значения стандартного отклонения повторяемости и внутри лабораторной воспроизводимости не превысили 3,4 и 5,9 % соответственно, величины смещения изменялись от –8,2 до 5,6 %, оценки расширенной неопределенности результатов составили от 12 до 16 % (Р = 0,95). Также в процессе валидации были оценены инструментальный предел определения, общая эффективность процесса и устойчивость метода.

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.

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The authors declare that there are no conflicts of interest present.