Rapid Mass Spectrometric Study of a Supercritical CO2-extract from Woody Liana Schisandra chinensis by HPLC-SPD-ESI-MS/MS

Woody liana Schisandra chinensis contains valuable lignans, which are phenylpropanoids with valuable biological activity. Among green and selective extraction methods, supercritical carbon dioxide (SC-CO2) was shown to be the method of choice for the recovery of these naturally occurring compounds. Carbon dioxide (CO2) was the solvent with the flow rate (10−25 g/min) with 2% ethanol as co-solvent. In this piece of work operative parameters and working conditions were optimized by experimenting with different pressures (200–400 bars) and temperatures (40–60 °C). The extraction time varied from 60 to 120 min. HPLC-SPD-ESI -MS/MS techniques were applied to detect target analytes. Twenty-six different lignans were identified in the S. chinensis SC-CO2 extracts

Polyphenols of <i>Perilla frutescens</i> of the family Lamiaceae identified by tandem mass spectrometry

Perilla frutescens is mainly cultivated as an oilseed crop. Perilla seeds contain 40–53 % of oil, 28 % of protein. The growing season is 100–150 days. In Russia, perilla is grown in the Far East, where the yield is 0.8–1.2 t/ha. Perilla of different geographical origin has its own special, sharply different features that characterize two geographical groups: Japanese and Korean-Chinese. These groups differ from each other in the length of the growing season, the height of plants, the color of the stem, the surface and the size of the leaves, the shape of the bush, the shape and size of the inflorescences, the size of the cups, the size and color of the seeds. P. frutescens contains a large number of polyphenolic compounds that are biologically active components. The purpose of this research was a metabolomic study of extracts from leaves of P. frutescens obtained from the collection of Federal Research Center the N.I. Vavilov All-Russian Institute of Plant Genetic Resources, grown on the fields of the Far East Experiment Station – Branch of Federal Research Center (Primorsky Krai, Russia). To identify target analytes in extracts, HPLC was used in combination with an ion trap. Preliminary results showed the presence of 23 biologically active compounds corresponding to P. frutescens. In addition to the reported metabolites, a number of metabolites were newly annotated in P. frutescens. There were hydroxycoumarin Umbelliferone; triterpene Squalene; omega-3 fatty acid Stearidonic [Moroctic] acid; higher-molecular-weight carboxylic acid: Tetracosenoic acid and Salvianic acid C; lignan Syringaresinol and cyclobutane lignan Sagerinic acid, etc. A wide range of biologically active compounds opens up rich opportunities for the creation of new drugs and dietary supplements based on extracts of perilla of the family Lamiaceae, subfamily Lamioideae, tribe Satureji and subtribe Perillinae

CHEMICAL STUDY OF SNOW OF VLADIVOSTOK CITY AND RUSSKY ISLAND

In the paper thefirst results of mass and spectrometer research of snow cover of the largest city in the Far East - Vladivostok (mainland and Island Russky), dropped-out on the November 19 2012, are presented. To exclude secondary pollution by anthropogenous aerosols we used the top layer (5-10 cm) of just dropped-out snow placed in the 3-liter sterile containers. In a couple of hours, when snow in containers thawed, 10 ml of liquid were gained from each sample and were analyzed on a mass spectrometer of high resolution with inductive-connected plasma (MS-ICP) Element XR (Thermo Scientific). Measurements were carried out with use of a technique of TsV3.18.05-2005 Fr.1.31.2005.01714. Tests were selected in 20 points: 16 points - Vladivostok, 3 points - Island Russky (DVFU campus, the bridge, the settlement) and a comparison point - the bay Hero in the southwest of Peter the Great Bay. For the first time application of the most highly sensitive chemical method for an applied ecological task is shown today. Distribution of Pb, Cr, Mn, Fe, Co, Ni, Cu and Zn in areas of Vladivostok different by anthropogenous loading and on Russian Island is revealed. In districts of Vladivostok with high transport loading high contents of metals (Mn, Cu, Zn) which source is motor transport (exhaustgases, autopaint, catalysts) are fixed also. Tests from districts of the Academic Town have traces of influence of the sea coast (halite and potassium-containing minerals) and railroad tracks (a microparticle of iron and its oxides) that strongly pollutes environment iron because of continuous movement of trains. In the tests taken on the Eagle hill, the highest point of Vladivostok, high concentrations of Mn (the highest concentration from all tests) and Cu (the third concentration from all tests) are recorded. This point of selection is in the downtown and, apparently, isn't ecologically clear. It should be noted that height above sea level in an urban environment isn't in sufficient condition for ecological safety. Russian Island is a pure zone with low background contents of heavy metals. The raised maintenance of Cu, Ni and Zn in snow cover of the bay Hero is shown

Исследование плодов образцов томата Solanum lycopersicum L., происходящих из разных климато-географических зон, и идентификация метаболитов методом тандемной масс-спектрометрии

Relevance. A number of scientific studies confirm that consumption of fruits and vegetables can reduce the risk of certain chronic diseases, such as cancer and cardiovascular diseases, for example, consumption of fresh tomatoes and tomato products is inversely proportional to the development of certain types of cancer. Tomato Solanum lycopersicum L. contains a large number of polyphenolic complexes, which are biologically active compounds. In this article, the authors have attempted for the first time to present the complete metabolomic composition of Solanum lycopersicum extracts.Materials and methods: As an object of research, authors used the extracts of Solanum lycopersicum L., from the collection of the Federal Research Center N.I. Vavilov All-Russian Institute of Plant Genetic Resources, grown and collected at the Far Eastern Experiment Station Branch of the Federal State Budgetary Scientific Institution in September 2020 (varieties: k-5351 Ont77 13, Canada; k-3149 Rehovoth, Israel; 2698 Ukraine). High performance liquid chromatography (HPLC) in combination with a BRUKER DALTONIKS ion trap (tandem mass spectrometry) was used to identify target analytes in extracts obtained by the maceration method.Discussion: The results of initial studies revealed the presence of 36 biologically active compounds, of which 22 were identified for the first time in Solanum lycopersicum L. These are Apigenin, Luteolin, Kaempferol, Taxifolin, Myricetin, Coutaric acid, Caffeoylmalic acid, Caftaric acid, Dicaffeoylquinic acid, coumarins Fraxetin, and Fraxetin-7-O-beta-glucuronide, Pelargonidin, Salvianolic acid D, Rosmanol, Colnelenic acid, Ethyl rosemary, lignan Medioresinol-O-hexoside, Squalene, etc. The findings will help to intensify future research into the development and production of various functional food products containing targeted extracts of Solanum lycopersicum L.Актуальность. Целый ряд научных исследований подтверждает, что потребление фруктов и овощей может снизить риск некоторых хронических заболеваний, таких как рак и сердечно- сосудистые заболевания, например, потребление свежих помидоров и продуктов из томатов обратно пропорционально развитию некоторых видов рака. Плоды томата Solanum lycopersicumL. содержат большое количество полифенольных комплексов, являющихся биологически активными соединениями. В данной статье авторы впервые попытались представить полный метаболомный состав экстрактов плодов Solanum lycopersicum.Материалы и методы: В качестве объекта исследования были использованы плоды томатов Solanum lycopersicum L. из коллекции Всероссийского института генетических ресурсов им. Н.И. Вавилова, выращенные и собранные на Дальневосточной опытной станции Филиале ВИР в сентябре 2020 года (сорта: к-5351 Ont77 13, Канада; к-3149 Rehovoth, Израиль; 2698 Украина). Для идентификации целевых аналитов в экстрактах, полученных мацерационным методом, использована высокоэффективная жидкостная хроматография (ВЭЖХ) в комплексе с ионной ловушкой BRUKER DALTONIKS (тандемная масс-спектрометрия).Результаты: Результаты начальных исследований выявили присутствие 36 полифенольных соединений и соединений других классов, из них 22 идентифицировано впервые в Solanum lycopersicumL. Это апигенин, лютеолин, кампферол, таксифолин, мирицетин, кутаровая кислота, кофеилмалевая кислота, кафтаровая кислота, дикаффеоилхиновая кислота, кумарины фраксетин и глюкоронид фраксетина, антоцианин пеларгонидин, сальвианоловая кислота D, розманол, колнеленовая кислота, этил розмаринат, лигнан медиоресинол, сквален и др. Полученные данные помогут интенсифицировать будущие исследования по разработке и производству различных продуктов функционального питания, содержащих целевые экстракты Solanum lycopersicumL

Zostera marina L.: Supercritical CO2-extraction and mass spectrometric characterization of chemical constituents recovered from seagrass

Three types of Zostera marina L. collection were extracted using the supercritical CO2-extraction method. For the purposes of supercritical CO2-extraction, old seagrass ejection on the surf edge, fresh seagrass ejection on the surf edge and seagrass collected in water were used. Several experimental conditions were investigated in the pressure range 50-350 bar, with the used volume of co-solvent ethanol in the amount of 1% in the liquid phase at a temperature in the range of 31-70 degrees C. The most effective extraction conditions are: pressure 250 Bar and temperature 60 degrees C for Z. marina collected in sea water. Z. marina contain various phenolic compounds and sulfated polyphenols with valuable biological activity. Tandem mass-spectrometry (HPLC-ESI-ion trap) was applied to detect target analytes. 77 different biologically active components have been identified in Z. marina supercritical CO2-extracts. 38 polyphenols were identified for the first time in Z. marina

Dracocephalum palmatum S. and Dracocephalum ruyschiana L. originating from Yakutia : a high-resolution mass spectrometric approach for the comprehensive characterization of phenolic compounds

Dracocephalum palmatum S. and Dracocephalum ruyschiana L. contain a large number of target analytes, which are biologically active compounds. High performance liquid chromatography (HPLC) in combination with an ion trap (tandem mass spectrometry) was used to identify target analytes in extracts of D. palmatum S. and D. ruyschiana L. originating from Yakutia. The results of initial studies revealed the presence of 114 compounds, of which 92 were identified for the first time in the genus Dracocephalum. New identified metabolites belonged to 17 classes, including 16 phenolic acids and their conjugates, 18 flavones, 5 flavonols, 2 flavan-3-ols, 1 flavanone, 2 stilbenes, 10 anthocyanins, 1 condensed tannin, 2 lignans, 6 carotenoids, 3 oxylipins, 2 amino acids, 3 sceletium alkaloids, 3 carboxylic acids, 8 fatty acids, 1 sterol, and 3 terpenes, along with 6 miscellaneous compounds. It was shown that extracts of D. palmatum are richer in the spectrum of polyphenolic compounds compared with extracts of D. ruyschiana, according to a study of the presence of these compounds in extracts, based on the results of mass spectrometric studies

Identification and Spatial Distribution of Bioactive Compounds in Seeds Vigna unguiculata (L.) Walp. by Laser Microscopy and Tandem Mass Spectrometry

The research presents a comparative metabolomic study of extracts of Vigna unguiculata seed samples from the collection of the N.I. Vavilov All-Russian Institute of Plant Genetic Resources. Analyzed samples related to different areas of use in agricultural production, belonging to different cultivar groups sesquipedalis (vegetable accessions) and unguiculata (grain accessions). Metabolome analysis was performed by liquid chromatography combined with ion trap mass spectrometry. Substances were localized in seeds using confocal and laser microscopy. As a result, 49 bioactive compounds were identified: flavonols, flavones, flavan-3-ols, anthocyanidin, phenolic acids, amino acids, monocarboxylic acids, aminobenzoic acids, fatty acids, lignans, carotenoid, sapogenins, steroids, etc. Steroidal alkaloids were identified in V. unguiculata seeds for the first time. The seed coat (palisade epidermis and parenchyma) is the richest in phenolic compounds. Comparison of seeds of varieties of different directions of use in terms of the number of bioactive substances identified revealed a significant superiority of vegetable accessions over grain ones in this indicator, 36 compounds were found in samples from cultivar group sesquipedalis, and 24 in unguiculata. The greatest variety of bioactive compounds was found in the vegetable accession k-640 from China

Rosa davurica Pall., Rosa rugosa Thumb., and Rosa acicularis Lindl. originating from Far Eastern Russia: Screening of 146 chemical constituents in three species of the genus Rosa

Rosa rugosa Thumb., Rosa davurica Pall., and Rosa acicularis Lindl. contain a large number of target analytes which are bioactive compounds. High performance liquid chromatography (HPLC), in combination with the ion trap (tandem mass spectrometry), was used to identify target analytes in MeOH extracts of R. rugosa, R. davurica, and R. acicularis, originating from the Russian Far East, Trans-Baikal Region, and Western Siberia. The results of initial studies revealed the presence of 146 compounds, of which 115 were identified for the first time in the genus Rosa (family Rosaceae). The newly identified metabolites belonged to 18 classes, including 14 phenolic acids and their conjugates, 18 flavones, 7 flavonols, 2 flavan-3-ols, 2 flavanones, 3 stilbenes, 2 coumarins, 2 lignans, 9 anthocyanins, 3 tannins, 8 terpenoids, 3 sceletium alkaloids, 4 fatty acids, 2 sterols, 2 carotenoids, 3 oxylipins, 3 amino acids, 5 carboxylic acids, etc. The proven richness of the bioactive components of targeted extracts of R. rugosa, R. davurica, and R. acicularis invites extensive biotechnological and pharmaceutical research, which can make a significant contribution both in the field of functional and enriched nutrition, and in the field of cosmetology and pharmacy

Phytochemical Analysis of Phenolics, Sterols, and Terpenes in Colored Wheat Grains by Liquid Chromatography with Tandem Mass Spectrometry

The colored grain of wheat (Triticum aestivum L.) contains a large number of polyphenolic compounds that are biologically active ingredients. The purpose of this work was a comparative metabolomic study of extracts from anthocyaninless (control), blue, and deep purple (referred to here as black) grains of seven genetically related wheat lines developed for the grain anthocyanin pigmentation trait. To identify target analytes in ethanol extracts, high-performance liquid chromatography was used in combination with Bruker Daltonics ion trap mass spectrometry. The results showed the presence of 125 biologically active compounds of a phenolic (85) and nonphenolic (40) nature in the grains of T. aestivum (seven lines). Among them, a number of phenolic compounds affiliated with anthocyanins, coumarins, dihydrochalcones, flavan-3-ols, flavanone, flavones, flavonols, hydroxybenzoic acids, hydroxycinnamic acids, isoflavone, lignans, other phenolic acids, stilbenes, and nonphenolic compounds affiliated with alkaloids, carboxylic acids, carotenoids, diterpenoids, essential amino acids, triterpenoids, sterols, nonessential amino acids, phytohormones, purines, and thromboxane receptor antagonists were found in T. aestivum grains for the first time. A comparative analysis of the diversity of the compounds revealed that the lines do not differ from each other in the proportion of phenolic (53.3% to 70.3% of the total number of identified compounds) and nonphenolic compounds (46.7% to 29.7%), but diversity of the compounds was significantly lower in grains of the control line. Even though the lines are genetically closely related and possess similar chemical profiles, some line-specific individual compounds were identified that constitute unique chemical fingerprints and allow to distinguish each line from the six others. Finally, the influence of the genotype on the chemical profiles of the wheat grains is discussed