This article presents results of the chemical composition study of the seeds oils lipid complex of Nigella Sativa L. grown under various geographic conditions. The task of the comprehensive study of the chemical composition of the plant and its individual parts remains relevant due to the wide spectrum of its pharmacological activity.The aim of this work is a comparative study of the fatty acid composition, a non-saponifiable fraction and the composition of essential oils of Nigella Sativa L. seeds grown in different regions of the world.Materials and methods. The combination of chromatography-mass spectrometry and 1H-NMR spectroscopy methods made it possible to study the qualitative and quantitative composition of Nigella Sativa L. lipid complex seeds. All the experiments were carried out in accordance with the requirements of the State Pharmacopoeia, 14th Ed, given in the corresponding general pharmacopeial monographs.Results. Profiles have been established and the content of fatty acids, sterines, triterpene alcohols, essential oils and thymoquinone found out in the lipid complex, has been estimated. The saponifiable portion of the complex is represented by triglycerides (81.7–95.3%), di(3.9–15.2%) and monoglycerides (0.7–4.1%). They mainly contain linoleic (55.8–60.6%), oleic (21.8–24.6%), palmitic (10.0–12.8%), stearic (2.4–3.2 %) and cis-11.14-eicosadiene (2.3–2.6%) acids. In the lipid complex, the contents of sterines and triterpene alcohols were 0.4–0.7%; up to 70% of the fraction was represented by β-sitosterol (22.5–29.2%), cycloartenol (20.1–36.6%) and 24 methylenecycloartanol (9.5–19.9%). In the trace amounts (up to 1.0%), cholesterol has been detected in all the samples. In the lipid complexes, the content of thymoquinone ranged from 0.7 to 2.6%.Conclusion. A comparative study of the seeds lipid complex of Nigella Sativa L. grown under various geographic conditions, has been carried out. The marker compounds as well as their content standards for determining the authenticity of raw materials (thymoquinone, para-cimen, cis-11.14-eicosadienic acid), have been identified.

The potentials of using a graphite matrix for laser desorption/ionization from a thin-layer chromatography (TLC) spot is studied. Using a series of pharmaceutical substances with various functional groups and synthetic N-heterocyclic compounds, it was shown that the simple application of graphite onto TLC spots (outlining contour of the spots and shading the spots with a pencil lead) ensured the efficient desorption/ionization of analytes. In most of cases, the recorded mass spectra revealed only [M + Na]⁺ and [M + K]⁺ ion peaks, doublets of which can be used to determine molecular masses. The appearance of [M + H]⁺ ion peaks in some mass spectra may be due to the presence of mineral acids in the samples. The described approach to the application of the “matrix” onto analyte spots eliminates the danger of spot blurring by a solution or an organic matrix, simplifies the procedure, and shortens the time of sample preparation.

The roots and rhizomes of Rubia tinctorum L. have been widely used both for industrial and medicinal purposes for centuries. The primary biologically active substances from Rubia tinctorum L. roots and rhizomes are anthraquinone derivatives such as ruberythric acid and lucidin-3-primeveroside. Their identification and quantification are carried out by various analytical methods, requiring a complicated sample preparation as well as special reagents and reference samples. However, NMR spectroscopy has no limitations of this kind. In this work, we have developed and validated a new express and standard-free method for the qualitative and quantitative analysis of ruberythric acid and lucidin-3-primeveroside by ¹H NMR spectroscopy in the extracts from the roots and rhizomes of Rubia tinctorum L. In this work, we have optimized the conditions of the sample preparation and registration of ¹H NMR spectra, determined the optimal solvent and reference compound and confirmed the obtained results by HPLC-UV-MS.