pmedpharmФармация и фармакологияPharmacy & Pharmacology2307-92662413-2241Pyatigorsk Medical and Pharmaceutical Institute - branch of Volgograd State Medical Univer10.19163/2307-9266-2024-12-2-117-130pmedpharm-1545Research ArticleОРИГИНАЛЬНАЯ СТАТЬЯRESEARCH ARTICLEРазработка и валидация методики количественного определения α-соланина, α-чаконина, соланидина в экстрактах из кожуры клубней картофеля клубненосного методом высокоэффективной жидкостной хроматографии и тандемной масс-спектрометрииDevelopment and validation of methods for quantitative determination of α-solanine, α-chaconine, solanidine in extracts from potato tuber peels BY High-performance liquid chromatography–tandem mass spectrometryhttps://orcid.org/0000-0002-7916-2269ОстриковаТ. О.OstrikovaT. O.

ассистент кафедры фармацевтической химии и фармакогнозии ФГБОУ ВО РязГМУ Минздрава России.

390026, Россия, г. Рязань, ул. Высоковольтная, д. 9

assistant of the Department of Pharmaceutical Chemistry and Pharmacognosy of Ryazan State Medical University n.a. I.P. Pavlov.  

9 Vysokovoltnaya Str., Ryazan, Russia, 390026

tostrikova0@gmail.comhttps://orcid.org/0000-0002-3268-4174БогомоловН. Г.BogomolovN. G.

студент 5-го курса фармацевтического факультета ФГБОУ ВО РязГМУ Минздрава России.

390026, Россия, г. Рязань, ул. Высоковольтная, д. 9.

5th year student of the Faculty of Pharmacy of Ryazan State Medical University n.a. I.P. Pavlov. 

9 Vysokovoltnaya Str., Ryazan, Russia, 390026

nikita.bogomolov50@gmail.comhttps://orcid.org/0000-0001-7829-2494МыльниковП. Ю.MylnikovP. Yu.

кандидат биологических наук, ассистент кафедры фармакологии с курсом фармации ФДПО ФГБОУ ВО РязГМУ Минздрава России. 

390026, Россия, г. Рязань, ул. Высоковольтная, д. 9.

Candidate of Sciences  (Biology), Assistant of the Department of Pharmacology with a course of pharmacy, Faculty of Additional Professional Education of Ryazan State Medical University n.a. I.P. Pavlov. 

9 Vysokovoltnaya Str., Ryazan, Russia, 390026

Pavelmylnikov@mail.ruhttps://orcid.org/0000-0003-1688-0017ЩулькинА. В.ShchulkinA. V.

доктор биологических наук, доцент, профессор кафедры фармакологии с курсом с курсом фармации ФДПО ФГБОУ ВО РязГМУ Минздрава России.

390026, Россия, г. Рязань, ул. Высоковольтная, д. 9.

Doctor of Sciences (Biology), Associate Professor, Professor of the Department of Pharmacology with a Course of Pharmacy, Faculty of Additional Professional Education of Ryazan State Medical University n.a. I.P. Pavlov. 

9 Vysokovoltnaya Str., Ryazan, Russia, 390026

alekseyshulkin@rambler.ruhttps://orcid.org/0000-0002-5618-7607ЧерныхИ. В.ChernykhI. V.

доктор биологических наук, доцент, заведующий кафедрой фармацевтической химии и фармакогнозии ФГБОУ ВО РязГМУ Минздрава России. 

390026, Россия, г. Рязань, ул. Высоковольтная, д. 9.

Candidate of Sciences (Biology), Associate Professor, Head of the Department of Pharmaceutical Chemistry of Ryazan State Medical University n.a. I.P. Pavlov. 

9 Vysokovoltnaya Str., Ryazan, Russia, 390026

ivchernykh88@mail.ruФедеральное государственное бюджетное образовательное учреждение высшего образования «Рязанский государственный медицинский университет имени академика И.П. Павлова» Министерства здравоохранения Российской ФедерацииРоссияRyazan State Medical University named after academician I.P. PavlovRussian Federation202425112024122117130Copyright © Острикова Т.О., Богомолов Н.Г., Мыльников П.Ю., Щулькин А.В., Черных И.В., 20242024Острикова Т.О., Богомолов Н.Г., Мыльников П.Ю., Щулькин А.В., Черных И.В.Ostrikova T.O., Bogomolov N.G., Mylnikov P.Y., Shchulkin A.V., Chernykh I.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.pharmpharm.ru/jour/article/view/1545

Перспективными метаболитами картофеля клубненосного (Solanum tuberosum L., сем. Solanaceae) являются α-соланин, α-чаконин и их агликон соланидин.

Цель

Цель. Разработка и валидация методики количественного анализа α-соланина, α-чаконина и соланидина в сухих экстрактах из кожуры клубней картофеля клубненосного методом высокоэффективной жидкостной хроматографии с тандемным масс-селективным детектированием (ВЭЖХ/МС/МС).

Материалы и методы

Материалы и методы. Анализ выполнялся в градиентном режиме на хроматографе «Ultimate 3000» (ThermoFisher, США) с тандемным масс-селективным детектором TSQ Fortis и колонкой UCT Selectra C18 4,6 мм×100 мм,  3 мкм, 100 Å. В работе использовался электроспрей в положительном режиме ионизации. Для количественного анализа применялись следующие переходы масс: α-соланин – 868,4→398,3 m/z; α-чаконин – 853,4→706,3 m/z;  соланидин − 398,3→98,1 m/z. Переходы масс для внутреннего стандарта фексофенадина: 502,3→171 m/z и 502,3→466,2 m/z. Время анализа составило 10 мин. Разработанные условия хроматографирования были проверены на пригодность. Валидацию проводили по следующим параметрам: специфичность, аналитическая область, линейность, правильность, прецизионность и нижний предел количественного определения.

Результаты

Результаты. Процедура валидации показала, что методика была селективной, достаточно чувствительной в отношении α-соланина, α-чаконина и соланидина (нижний предел количественного определения составил соответственно 50, 10 и 2 нг/мл), линейна в интервале концентраций соответственно 50–5000, 10–5000 и 2–100 нг/мл, обладала удовлетворительной правильностью (RSD не превышали 7% для каждого из веществ), достаточной презиционностью (для α-соланина RSD не превышало 5%, для α-чаконина, соланидина – не более 10%).

Заключение

Заключение. Разработана и валидирована методика количественного определения α-соланина, α-чаконина и соланидина в сухих экстрактах, полученных из кожуры клубней картофеля клубненосного, методом ВЭЖХ-МС/МС. Данная методика может быть использована в рутинной практике количественного определения гликоалкалоидов при анализе их содержания в пищевых продуктах и комбинированных лекарственных средствах.

Promising metabolites of potato tuberosum (Solanum tuberosum L., f. Solanaceae) are α-solanine, α-chaconine and their aglycone solanidine.

The aim of the work was to develop and validate methods for a quantitative analysis of α-solanine, α-chaconine and solanidine in dry extracts from the potato tuber peels by a high-performance liquid chromatography with a tandem  mass-selective detection (HPLC/MS/MS).

Materials and methods

Materials and methods. The analysis was performed in a gradient mode on an Ultimate 3000 chromatograph (ThermoFisher, USA) with a TSQ Fortis tandem mass-selective detector and a 4.6 mm×100 mm, 5 μm, 100 Å UCT Selectra C18 column. An electrospray in a positive ionization mode was used in this work. The following mass transitions were used for the quantitative analysis: α-solanine, 868.4→398.3 m/z; α-chaconine, 853.4→706.3 m/z; solanidine, 398.3→98.1 m/z. The following mass transitions were used for the internal standard fexofenadine: 502.3→171 m/z and 502.3→466.2 m/z. The analysis time was 10 min. The developed chromatography conditions were validated for a suitability. The validation was performed according to the following parameters: specificity, analytical range, linearity, correctness, precision and a lower limit of quantification.

Results

Results. The validation procedure showed that the methodology was selective, sufficiently sensitive for α-solanine, α-chaconine and solanidine (lower limits of the quantification were 50, 10 and 2 ng/mL, respectively), the linear in the concentration range of 50–5000, 10–5000 and 2–100 ng/mL, respectively; it was satisfactorily correct (RSD did not  exceed 7% for each of the substances) and sufficiently sensitive (RSD for α-solanine did not exceed 5%, for α-chaconine and solanidine – not more than 10%).

Conclusion

Conclusion. A technique for a quantitative determination of α-solanine, α-chaconine and solanidine in dry extracts obtained from potato tuber peels by HPLC/MS/MS has been developed and validated. This technique can be used in the routine practice of the glycoalkaloids quantitative determination when analyzing their content in food products and combination medicines.

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