zldmЗаводская лаборатория. Диагностика материаловIndustrial laboratory. Diagnostics of materials1028-68612588-0187ООО «Издательство «ТЕСТ-ЗЛ»10.26896/1028-6861-2025-91-11-5-12zldm-2652Research ArticleАНАЛИЗ ВЕЩЕСТВАSUBSTANCES ANALYSISПрименение газовой хромато-масс-спектрометрии для обнаружения примесей в хлорогеновой и кофейной кислотахApplication of gas chromatography-mass spectrometry for the detection of impurities in chlorogenic and caffeic acidsКсенофонтоваТ. Д.KsenofontovaT. D.

Татьяна Дмитриевна Ксенофонтова

119991, Москва, Ленинский просп., д. 31; 119049, Москва, Ленинский просп., д. 4.

Tatyana D. Ksenofontova 

31, Leninsky prosp., Moscow, 119991; 4, Leninsky prosp., Moscow, 119049

 

Ksenofontovat@bk.ruБарановскаяВ. БBaranovskaiaV. B.

Василиса Борисовна Барановская

119991, Москва, Ленинский просп., д. 31; 119049, Москва, Ленинский просп., д. 4.

Vasilisa B. Baranovskaia 

31, Leninsky prosp., Moscow, 119991; 4, Leninsky prosp., Moscow, 119049

Институт общей и неорганической химии им. Н. С. Курнакова РАН; Национальный исследовательский технологический университет «МИСИС»РоссияKurnakov Institute of General and Inorganic Chemistry, RAS; National University of Science and Technology «MISIS»Russian Federation2025261120259111512Copyright © Ксенофонтова Т.Д., Барановская В.Б., 20252025Ксенофонтова Т.Д., Барановская В.Б.Ksenofontova T.D., Baranovskaia V.B.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/2652

Природное происхождение и склонность к деградации при хранении гидроксикоричных кислот, широко используемых в фармацевтической и пищевой промышленности, обуславливают необходимость контроля их качества, в частности, определение примесей и продуктов деградации. Рассмотрены возможности газовой хромато-масс-спектрометрии (ГХ-МС) для анализа чистых образцов кофейной и хлорогеновой кислот для обнаружения примесей различной природы. Показано, что ГХ-МС-анализ кислот без дериватизации невозможен ввиду высокой полярности и термической нестабильности исследуемых соединений, что приводит к их разложению в условиях хроматографирования. Для повышения летучести и термостабильности проведена дериватизация с использованием N,O-бис(триметилсилил)трифторацетамида в присутствии триметилхлорсилана, что позволило повысить чувствительность метода. Анализ масс-спектров дериватизированных образцов с применением библиотечного поиска выявил присутствие различных производных коричной кислоты, а также неидентифицированного пика, предположительно соответствующего триметилсилильному производному тригидроксикоричной кислоты. Полученные результаты демонстрируют эффективность метода ГХ-МС с предварительной дериватизацией для анализа чистых гидроксикоричных кислот и подтверждают целесообразность его применения для контроля качества и изучения стабильности подобных соединений.

Hydroxycinnamic acids, including caffeic and chlorogenic acids, are widely found in plant extracts and demonstrate significant biological activity, making them promising for pharmaceutical and food industry applications. However, their natural origin and tendency to degrade during storage requires quality control, including the identification of impurities and degradation products. This study explores the potential of gas chromatography – mass spectrometry (GC-MS) for the analysis of pure caffeic and chlorogenic acid samples in order to detect impurities of various origins. It demonstrates that GC-MS analysis of acids without derivatization is not feasible due to the high polarity and thermal instability of the compounds under study, which leads to their decomposition under chromatography conditions. To improve volatility and thermal stability, derivatization was performed using N,O-bis(trimethylsilyl)trifluoroacetamide in the presence of trimethylchlorosilane, which increased the method’s sensitivity. Mass spectral analysis of the derivatized samples, supported by library searches, revealed the presence of various cinnamic acid derivatives, as well as an unidentified peak, presumably corresponding to the trimethylsilyl derivative of trihydroxycinnamic acid. The results demonstrate the effectiveness of GC-MS with prior derivatization for the detailed analysis of pure hydroxycinnamic acids and confirm its suitability for quality control and stability studies of these compounds.

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