zldmЗаводская лаборатория. Диагностика материаловIndustrial laboratory. Diagnostics of materials1028-68612588-0187ООО «Издательство «ТЕСТ-ЗЛ»10.26896/1028-6861-2025-91-11-13-25zldm-2653Research ArticleАНАЛИЗ ВЕЩЕСТВАSUBSTANCES ANALYSISАнализ биологических жидкостей и шерсти животных на содержание бета-адреностимуляторов методом хромато-масс-спектрометрииAnalysis of biological fluids and animal hairs for beta-adrenergic agonists by liquid chromatography – mass-spectrometryСорокинА. В.SorokinA. V.

Александр Валерьевич Сорокин

123022, Москва, Звенигородское ш., д. 5

Alexander V. Sorokin

5, Zvenigorodskoe sh., Moscow, 123022

alex_sorokin@list.ruЖедуловА. Е.ZhedulovA.

Александр Евгеньевич Жедулов 

123022, Москва, Звенигородское ш., д. 5

Alexander E. Zhedulov 

5, Zvenigorodskoe sh., Moscow, 123022

Всероссийский государственный центр качества и стандартизации лекарственных средств для животных и кормовРоссияThe Russian State Center for Animal Feed and Drug Standardization and QualityRussian Federation20252611202591111325Copyright © Сорокин А.В., Жедулов А.Е., 20252025Сорокин А.В., Жедулов А.Е.Sorokin A.V., Zhedulov A.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/2653

Для контроля выведения бета-адреностимуляторов, применяемых в целях ускорения роста мышечной массы в животноводстве, разработана методика хромато-масс-спектрометрического определения 20 соединений данного ряда в моче и крови, а также 12 соединений в образцах шерсти крупного рогатого скота (КРС). Пробоподготовка образцов мочи КРС включает ферментативный гидролиз в среде фосфатного буферного раствора и очистку методом твердофазной экстракции на сорбенте Copure C8/SCX. Из образцов крови определяемые соединения извлекали ацетонитрилом в присутствии уксусной кислоты; проводили высаливание и дисперсионную очистку экстракта, используя C18 и оксид алюминия. Образцы шерсти подвергали щелочному гидролизу, определяемые соединения извлекали метил-трет-бутиловым эфиром с последующим переведением в ацетонитрил и проводили дисперсионную очистку экстракта. Общие потери бета-адреностимуляторов в процессе пробоподготовки образцов крови составляли 27 – 85 %, образцов мочи — 2 – 80 % в зависимости от аналита. Хроматографическое разделение осуществляли в градиентном режиме на колонке ACQUITY UPLC HSS C18, детектирование проводили в режиме мониторинга выбранных реакций с регистрацией не менее двух ионов-продуктов для каждого определяемого соединения. Диапазоны определяемых содержаний бета-адреностимуляторов в моче составили от 0,25 до 20,0 мкг/кг, в крови — от 0,1 до 10,0 мкг/кг, в шерсти — от 0,5 до 20,0 мкг/кг в зависимости от аналита. Значения относительной расширенной неопределенности при анализе мочи и крови находятся в диапазоне от 9 до 25 %, шерсти — от 9 до 30 %.

To control the excretion of beta-agonists used to accelerate the growth of muscle mass in animal husbandry, a method of determination of 20 compounds of this series in the cattle urine and blood, and 12 compounds in the cattle hairs samples by high-performance liquid chromatography – tandem mass spectrometry has been developed. The sample preparation of cattle urine included enzymatic hydrolysis in a phosphate buffer followed by purification using solid-phase extraction with a Copure C8/SCX sorbent. For the blood samples extraction of analytes by acetonitrile and acetic acid, followed by a phase separation and purification using C18 and aluminum oxide were carried out. Hair samples were subjected to an alkaline hydrolysis, and the analytes were extracted using methyl tert butyl ether. The extract was then transferred to acetonitrile for further dispersive purification. The overall loss during sample preparation ranged from 27 to 85% for blood samples and from 2 to 80% for urine samples, depending on the compound being determined. Chromatographic separation was conducted in a gradient mode using an ACQUITY UPLC HSS C18 column. Detection was performed in the selected reactions monitoring mode with registration of at least two product ions for each compound. The detection ranges of beta-agonists in urine were 0.25 – 20.0 μg/kg; 0.1 – 10.0 μg/kg in blood; 0.5 – 20.0 μg/kg in hairs depending on the analyte. For urine and blood analysis, the relative expanded uncertainty values ranged from 9 to 25%, while for hair analysis, they ranged from 9 to 30%.

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