zldmЗаводская лаборатория. Диагностика материаловIndustrial laboratory. Diagnostics of materials1028-68612588-0187ООО «Издательство «ТЕСТ-ЗЛ»10.26896/1028-6861-2023-89-9-13-24zldm-2009Research ArticleАНАЛИЗ ВЕЩЕСТВАSUBSTANCES ANALYSISПрямое определение глифосата и его метаболита в растительном сырье и объектах окружающей среды методом хромато-масс-спектрометрииDirect determination of glyphosate and its metabolite in the plant raw material and environmental objects by chromatography-mass spectrometryСорокинА. В.SorokinA. V.

Александр Валерьевич Сорокин

123022, Москва, Звенигородское ш., д. 5

Alexander V. Sorokin

5, Zvenigorodskoe shosse, Moscow, 123022

alex_sorokin@list.ruВсероссийский государственный центр качества и стандартизации лекарственных средств для животных и кормов (ФГБУ «ВГНКИ»)РоссияThe Russian State Center for Animal Feed and Drug Standardization and Quality (FGBU «VGNKI»)Russian Federation2023240920238991324Copyright © Сорокин А.В., 20232023Сорокин А.В.Sorokin A.V.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://www.zldm.ru/jour/article/view/2009

Глифосат является популярным гербицидом и часто применяется для десикации культурных растений в целях ускорения их созревания. Применение препаратов на его основе приводит к загрязнению сельскохозяйственной продукции, почвы, поверхностных и подземных вод. Для контроля его остаточного содержания разработана методика, позволяющая определять глифосат и аминометилфосфоновую кислоту (АМФК) без предварительной дериватизации. Методика характеризуется относительно простой и экономичной процедурой пробоподготовки. Из образцов сырья растительного происхождения аналиты извлекают уксуснокислым раствором метанола в воде в присутствии динатриевой соли ЭДТА (ЭДТА-Na2) и дихлорметана; из образцов воды — в присутствии ЭДТА-Na2 и уксусной кислоты; из образцов почвы — слабым раствором аммиака. Экстракты очищают методом твердофазной экстракции (ТФЭ) и осаждают белки ацетонитрилом. Диапазон определяемых содержаний глифосата и АМФК в сырье растительного происхождения составил 0,1 – 5,0 мг/кг, в поверхностных и подземных водах — 0,001 – 0,05 мг/л (глифосат) и 0,002 – 0,05 мг/л (АМФК), в почве и почвогрунтах — 0,02 – 0,8 мг/кг (глифосат) и 0,04 – 0,8 мг/кг (АМФК). Значения относительного стандартного отклонения находятся в диапазоне 1,8 – 19,5 % при степени извлечения определяемых соединений от 80,5 до 108,1 %. Достигнутые значения пределов определения (ПО) согласуются с установленными максимально допустимыми уровнями в ТР ТС 015/2011 и СанПиН 1.2.3685–21.

Glyphosate is a popular herbicide often used for desiccation of crops. The use of glyphosate-based chemicals leads to the contamination of agricultural products, soils, surface and groundwater. For safety control of raw materials of the plant origin and environmental objects, a technique based on the tandem chromato-mass-spectrometry was developed to provide for the quantitative determination of glyphosate and aminomethylphosphonic acid (AMPA) without prior derivatization. The technique is characterized by a relatively simple and cost-effective sample preparation procedure. The compounds are extracted from plant raw materials with an acetic acid solution of methanol in water, in the presence of 2-aqueous disodium salt of ethylenediamine-N,N,N’,N’-tetraacetic acid (EDTA-Na2) and dichloromethane. Extraction of analytes from water samples is carried out in the presence of EDTA-Na2 and acetic acid; whereas their extraction from soil samples is carried out with a weak solution of ammonia. The extracts are purified by solid phase extraction (SPE), and proteins are precipitated with acetonitrile. Linear-dynamic ranges of glyphosate and AMPA determination are characterized by calibration curves with correlation coefficients (R) ≥0.99. The working range of glyphosate and AMPA determination in raw materials of plant origin was from 0.1 to 5.0 mg/kg; in surface and ground water from 0.001 to 0.05 mg/liter (glyphosate) and from 0.002 to 0.05 mg/liter (AMPA); in soils from 0.02 to 0.8 mg/kg (glyphosate) and from 0.04 to 0.8 mg/kg (AMPA). The values of the relative standard deviation range from 1.8 to 19.5%, with recovery levels ranging from 80.5 to 108.1%. The achieved values of the determination limits are consistent with the maximum permissible levels indicated in TR CU 015/2011 and SanPiN 1.2.3685–21.

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