Isolation of ecdysterone from the roots ofRhaponticum carthamoides

The solubility of ecdysterone in individual solvents and mixtures has been studied. A method has been developed for isolating ecdysterone from the roots ofRhaponticum carthamoides. Extraction from the raw material was carried out with methanol. The catty oils and tanning and resinous substances were eliminated from the concentrated and water-diluted extract by treatment with chloroform. The combined ecdysteroids were extracted from the purified aqueous solution with chloroform-isopropanol (1:1). They were freed from pigments by chromatography on alumina (Brockmann activity grade II) with elution by methanol-chloroform (1:2). The product was recrystallized from methanol-ethyl acetate (1:9), giving 0.05% (on the weight of the raw material) of ecdysterone.Institute of the Chemistry of Plant Substances, Academy of Sciences of the Uzbek SSR, Tashkent. Translated from Khimiya Prirornykh Soedinenii, No. 4, pp. 528–529, July–August, 1980.     

Isolation of ecdysterone from the inflorescences ofRhaponticum integrifolium

A method has been developed for isolating ecdysterone from the inflorescences ofRh. integrifolium. The yield is 0.15% on the weight of the raw material.     

Isolation of ecdysterone

The kinetics of the extraction of ecdysterone from the roots with rhizomes ofRhaponticum carthamoides has been studied. The results of investigations on the selection of the optimum solvent for extracting ecdysterone from the raw material, for the process of sorption purification, and for the recrystallization of the ecdysterone are given.Institute of the Chemistry of Plant Substances, Academy of Sciences of the Uzbek SSR, Tashkent. Translated from Khimiya Prirodnykh Soedinenii, No. 5, pp. 601–605, September–October, 1983.     

Application of the chugaev reaction for the quantitative determination of ecdysones

Summary The spectrophotometric characteristics of the products of the Chugaev reaction with ecdysones have been studied. Methods have been proposed for determination of ecdysterone and viticosterone E in an artificial mixture and of ecdysterone in extracts of plant raw material by thin-layer chromatography followed by the Chugaev reaction.A. V. Palladin Institute of Biochemistry, Academy of Sciences of the Ukrainian SSR, Kiev. Translated from Khimiya Prirodnykh Soedinenii, No. 2, pp. 227–230, March–April, 1977.     

Isolation of ecdysterone from the inflorescences ofRhaponticum integrifolium

A method has been developed for isolating ecdysterone from the inflorescences ofRh. integrifolium. The yield is 0.15% on the weight of the raw material.Institute of the Chemistry of Plant Substances, Academy of Sciences of the Uzbek SSR, Tashkent. Translated from Khimiya Prirodnykh Soedinenii, No. 5, pp. 667–668, September–October, 1979.     

Phytoecdysteroids of plants of the genus Silene. XVII. Ecdysterone 22,25-di-O-benzoate from Silene scabrifolia

The new phytoecdysteroid ecdysterone 22,25-di-O-benzoate (IV) has been isolated from the epigeal organs ofSilene scabrifolia Kom. The alkaline hydrolysis of (IV) gave ecdysterone 25-O-benzoate and ecdysterone (I). Details of the IR, UV, mass, PMR, and¹³C NMR spectra of compound (IV) are given.     

Study of excretion of ecdysterone in human urine

A study of excretion in human urine of ecdysterone, which is the active component of several over-the-counter supplements such as "Ecdysten", reportedly used by athletes, is presented. The study was performed after oral administration of 20 mg of ecdysterone. The collected urine samples were prepared using the standard screening extraction procedure for the free and conjugated fraction of anabolic steroids, and analyzed by gas chromatography (GC) coupled with quadrupole mass spectrometry (MS) and also with high-resolution mass spectrometry (HRMS). Two ecdysterone metabolites were identified and detected along with unchanged ecdysterone. Accurate mass measurements were made for diagnostic ions, including the molecular ion of the main metabolite of ecdysterone, deoxyecdysone, which, to our knowledge, has not previously been reported in the literature. These accurate mass measurements support the proposed fragmentation scheme.     

A new approach to obtain Kevlar-49 from PET waste bottles

Non-biodegradable polyethylene terephthalate (PET) bottles have attracted increasing attention due to environmental concern in today’s world. In order to reduce the amount of solid wastes generated and the dependency on fossil resources, a new approach has been conducted to prepare Kevlar-49 from PET waste bottles. Terephthalic acid, the main raw material used for preparation of Kevlar, was regenerated from PET waste bottles via subjection to a saponification process, whereas p-phenylenediamine was prepared from PET waste bottles via the Hoffmann rearrangement method. Kevlar was synthesized from the reaction of terephthalic acid and p-phenylenediamine by polycondensation reaction. The structures of terephthalic acid, p-phenylenediamine and Kevlar were characterized by FT-IR, ¹H NMR, ¹³C NMR, and elemental analysis (CHN). In this study, thermogravimetric analysis and differential scanning calorimetry, X-ray diffraction (XRD), as well as the mechanical properties (tensile strength, modulus, and percentage elongation at break) of the synthesized Kevlar-49, were compared with commercial Kevlar-49, prepared from the same raw materials, for better understanding of their properties.     

Phytoecdysteroids of plants of the genus Silene. XVII. Ecdysterone 22,25-di-O-benzoate from Silene scabrifolia

The new phytoecdysteroid ecdysterone 22,25-di-O-benzoate (IV) has been isolated from the epigeal organs ofSilene scabrifolia Kom. The alkaline hydrolysis of (IV) gave ecdysterone 25-O-benzoate and ecdysterone (I). Details of the IR, UV, mass, PMR, and¹³C NMR spectra of compound (IV) are given.Institute of the Chemistry of Plant Substances, Uzbek SSR Academy of Sciences, Tashkent. Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 363–366, May–June, 1990.     

Phytoecdysteroids of plants of the genusSilene. III. Sileneoside A — A new glycosidic ecdysteroid ofSilene brachuica

Ecdysterone (I), viticosterone E, polypodine B, and integristerone A (II) have been isolated from the epigeal part of the plantSilene brachuica Boiss. In addition to substances (I) and (II), the phytoecdysteroid sileneoside A has been isolated from the root of this plant. It has been shown that sileneoside A is ecdysterone 22-O-α-D-galactoside.     

Obtaining Bioactive Compounds from the Coffee Husk (Coffea arabica L.) Using Different Extraction Methods

Coffee husks (Coffea arabica L.) are characterized by exhibiting secondary metabolites such as phenolic compounds, which can be used as raw material for obtaining bioactive compounds of interest in food. The objective of this study is to evaluate different methods for obtaining the raw material and extracting solutions of bioactive compounds from coffee husks. Water bath and ultrasound-assisted extraction methods were used, using water (100%) or ethanol (100%) or a mixture of both (1:1) as extracting solutions and the form of the raw material was in natura and dehydrated. The extracts were evaluated by their antioxidant potential using DPPH radicals, ABTS, and iron reduction (ferric reducing antioxidant power (FRAP)), and later total phenolic compounds, total flavonoids, and condensed tannins were quantified the phenolic majority compounds were identified. It was verified that the mixture of water and ethanol (1:1) showed better extraction capacity of the compounds with antioxidant activity and that both conventional (water bath) or unconventional (ultrasound) methods showed satisfactory results. Finally, a satisfactory amount of bioactive compounds was observed in evaluating the chemical composition (total phenolic compounds, total flavonoids, condensed tannins, as well as the analysis of the phenolic profile) of these extracts. Corroborating with the results of the antioxidant activities, the best extracting solution was generally the water and ethanol mixture (1:1) using a dehydrated husk and water bath as the best method, presenting higher levels of the bioactive compounds in question, with an emphasis on chlorogenic acid. Thus, it can be concluded that the use of coffee husk as raw material to obtain extracts of bioactive compounds is promising. Last, the conventional method (water bath) and the water and ethanol mixture (1:1) stood out among the methods and extracting solutions used for the dehydrated coffee husk.     

Phytoecdysteroids of plants of the genusSilene

Ecdysteroids produced by plants of the genusSilene are considered. The discussion covers 17 species of plants, from which 45 ecdysteroids have been isolated. It has been shown that ecdysterone is the most characteristic representative of the biosynthesis of ecdysteroids in theSilene series.     

Phytoecdysteroids of plants of the genusSilene. V. Sileneoside B — An ecdysterone digalactoside fromSilene brahuica

The phytoecdysteroid sileneoside B has been isolated from the roots ofSilene brahuica Boiss.; it is ecdysterone 3,22-di-O-α-D-galactopyranoside.     

祁州漏芦中蜕皮甾酮类化学成分的研究

从祁州漏芦的根中分离得到7个蜕皮甾酮化合物,采用近代光谱方法鉴定其为ajugasteroneC-2,3;20,22-diacetonide(1);25-deoxy-9(11)-dehydro-20-hydroxyecdysone-20,22-monoacetonide(2);ajugasteroneC-20,22-monoacetonide(3);ajugasteroneC(4);rhapontisteroneC(5);ecdysterone(6);11α-hydrox-yecdysteroneecdysterone(7).其中化合物1和2是在自然界中首次分离到的新化合物,化合物3是首次在祁州漏芦中分离得到的.     

Phytoecdysteroids of plants of the genusSilene. VII. Sileneoside D — ecdysterone 3-O-α-D-galactopyranoside fromSilene brahuica

A phytoecdysteroid, sileneoside D, has been isolated from the roots ofSilene brahuica Boiss. and it has been shown to be ecdysterone 3-O-α-D-galactopyranoside.     

LC–UV Method with Pre-Column Derivatization for the Determination of Ciclopirox Olamine in Raw Material and Topical Solution

A rapid, simple and sensitive liquid chromatographic method has been developed to assay ciclopirox olamine in raw material and topical solution. The analysis used a reversed-phase C₁₈ end-capped column, with UV detection at 305 nm and pre-column derivatization with dimethyl sulphate. A linear response (r ² > 0.999) was observed in the range of 0.4–200 μg mL^?1. The method showed good recoveries for the raw material and topical solution and the relative standard deviation intra and inter-day were ≤2.00%. Validation parameters such as specificity and robustness were also determined. The proposed method provided an accurate and precise analysis of ciclopirox olamine in raw material and topical solution.     

Study of the kinetics of the extraction of flavonoids from plant raw material I. Extraction of rutin fromSida hermaphrodita

The influence of the concentration of ethanol (50, 60, and 70%, of the degree of grinding of the plant raw material, and of the time of maceration, on the yield of rutin from the epigeal part ofVirginia sida, family Malvaceae has been studied. It has been established that the highest yield of rutin can be obtained from raw material ground to 2.5–3.0 mm with the use of 70% ethanol and a time of maceration of 12 h. In an investigation of the influence of the concentration of ethanol and the time of steeping on the yield of rutin from raw material ground to 2.5–2.0 mm, regression equations for 50, 60, and 70% ethanolic extractions have been derived.     

Certified calibration solution reference material for the determination of perfluorooctane sulfonate from the National Metrology Institute of Japan (NMIJ)

A new calibration solution reference material for the determination of perfluorooctane sulfonate anion (PFOS) and its salts has been issued as a certified reference material (CRM) by the National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). The purity amount-of-substance fraction of raw material potassium perfluorooctane sulfonate (K-PFOS) was evaluated based on the results obtained using the freezing point depression method, and the purity mass fraction of the raw material was calculated using the average molar mass of impurities, the molar mass of K-PFOS, and the purity amount-of-substance fraction. The certified concentration of this CRM was obtained by multiplying the dilution ratio of the raw material in a prepared solution (methanol) determined from the gravimetric blending method by the purity of the raw material. The preparation concentration of K-PFOS as a certified value of NMIJ CRM 4220-a was determined to be 9.93?mg?kg^?1. In addition, the standard uncertainty of the certified value was evaluated from the purity evaluation as well as from sample inhomogeneity, instability, and preparation variation obtained from LC/MS measurements of different gravimetrically prepared solutions of the NMIJ CRM. Consequently, the expanded uncertainty was estimated to be 0.15?mg?kg^?1 with a coverage factor k?=?2 corresponding to the half-width of estimated confidence interval of approximately 95%.     

The catalysis, synthesis and characterization of ferrocenylchalcone

Eight kinds of ferrocenylchalcone derivatives were synthesized by the reaction of acetylferrocene and aromatic aldehyde using solid as catalyst in the experiment. The influrence of the catalysts, the raw material molar ratios and reaction times on the yield of ferrocenylchalcone derivatives are discussed. The optimal conditions of synthesis reaction have been selected: the catalyst was KF/Al₂O₃, n(acetyl ferrocene)/n(formal dehyde) = 1:1.2. The structures of the products were characterized by melting point test, IR, ¹HNMR, ¹³CNMR and elemental analysis.     

Encapsulation of proteins by Electro Hydro Dynamic Atomization

Summary: Aerosol reactor for Electro Hydro Dynamic Atomization has been used to encapsulate water soluble proteins in poly(ε-caprolactone). As a raw material w/o emulsion of BSA water solution emulsified in the organic solution of polymer was applied. Stability of the spraying process itself for particles production was investigated. Also raw material emulsion stability has been examined and emulsion stabiliser has been found. Protein release rate from produced particles was determined.