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Objective To study the chemical constituents of Hippocampus trimaculatus Leach. Methods After extracted with ethanol, Hippocampus trimaculatus Leach was isolated and purified by silica gel column chromatography, Sephadex LH-20 gel column chromatography, and reversed-phase C18 column chromatography. The structures of compounds were identified by physical and chemical properties, spectral data and literature comparison. Results Eight compounds were isolated from Hippocampus trimaculatus Leach and identified as L-phenylalanine (1), alanine (2), inosine (3), cholesterol (4), N-acetyltyramine (5), uracil (6), D-mannitol (7), tetrodoine (8), respectively. Conclusion Compounds 5, 7, 8 are isolated from Hippocampus trimaculatus Leach for the first time.
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Fourteen flavonoids were isolated and purified from Epimedium sagittatum by various chromatography techniques such as macroporous adsorbent resin, silica gel, ODS, Sephadex LH-20, HW-40C and semi-preparative HPLC. Their structures were identified by analysis of physicochemical properties and spectral data, and determined as 3′-hydroxy-baohuoside-Ⅱ (1), huazhongilexone-7-O-β-D-glucopyranoside (2), kaempferol-3-O-α-L-rhamnoside (3), baohuoside-Ⅱ (4), icariside-Ⅱ (5), kaempferol 3,7-di-O-α-L-rhamnopyranoside (6), (+)-aromadendrin (7), kaempferol 3-O-(2-O-β-D-apiofuranosyl)-α-L-rhamnopyranoside (8), sagittatoside A (9), 2″-O-rhamnosyl icariside-II (10), apigenin-7-O-β-D-glucoside (11), quercetin 3-O-β-D-apiofuranoyl-(1→2)-α-L-rhamnopyranoside (12), kaempferol (13), icariin (14). Among them, compound 1 is a new compound, while compounds 2, 6-8, 11, and 12 were isolated from E.sagittatum for the first time.
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Alkaloids, widespread in plants, have a series of pharmacological activities and have been widely used to treat various diseases. Because alkaloids are usually presented in multicomponent mixtures and are deeply low in content, they are very difficult to extract and separate by traditional methods. High-speed counter current chromatography(HSCCC) is a kind of liquid-liquid chromatography without solid support phase, which has the advantages of large injection volume, low cost, and no irreversible adsorption. Compared with the traditional methods of extraction and separation of alkaloids, HSCCC can ensure the separation of many different alkaloids at one time, with a high recovery and large amount. In this paper, the advantages and disadvantages of HSCCC compared with traditional separation methods were discussed and the solvent system and elution mode of HSCCC used to separate alkaloids in recent years were summarized by referring to the relevant literature to provide some references for the separation of alkaloids by HSCCC.
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Biological Products , Countercurrent Distribution/methods , Chromatography, High Pressure Liquid/methods , Alkaloids/analysis , Solvents/chemistryABSTRACT
Paridis Rhizoma， a traditional valuable Chinese herbal medicine， has the functions of clearing heat and removing toxin， relieving edema and pain， cooling liver and calming convulsion， which can be used to treat various diseases such as mumps， abscess， burn， bleeding， and tumor. It has been used in folk medicine for a long time and is the main raw material of various Chinese patent medicines such as Gongxuening Capsules and Yunnan Baiyao. Polyphyllin Ⅰ， an isospirostanol saponin and one of the main active components in Paridis Rhizoma， is distributed in the rhizome， pericarp， and leaves of Paris polyphylla. With high polarity， polyphyllin Ⅰ is mainly extracted by n-butanol extraction and macroporous adsorption resin chromatography， separated by silica gel column chromatography and preparative high performance liquid chromatography， and purified with the combination of methods. With anti-tumor， anti-inflammatory， antibacterial， and anti-virus effects， it is generally employed to treat liver cancer， lung cancer， gastric cancer and other cancers as well as arthritis， influenza， sore toxin， and bacterial infection. However， polyphyllin Ⅰ may cause stomach irritation， hemolysis， liver damage， kidney damage， heart damage， and other adverse reactions. Pharmacokinetic studies show that it has problems such as low bioavailability and poor intestinal absorption and permeability， which affect the clinical application of polyphyllin Ⅰ. This paper summarizes the research on the plant sources， extraction and separation methods， pharmacological effects， adverse reactions， and pharmacokinetics of polyphyllin Ⅰ in recent years， which is expected to provide a reference for the rational clinical application and other in-depth research work of polyphyllin Ⅰ.
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One undescribed diterpenoid acid and six compounds were isolated from the 95% ethanol fraction of Pinus kesiya var. langbianensis (A.Chev.) Gaussen ex Bui resin by using various chromatographic methods, including MCI Gel, Sephadex LH-20, ODS, silica gel and semi-preparative HPLC. The planar structures were identified by spectroscopy methods (1D, 2D NMR, UV, IR, MS, etc.), and the absolute configuration of the new compound was determined by ECD calculation. Compound 1 is a new compound, and compounds 2, 5-7 were isolated from Pinus kesiya var. langbianensis (A.Chev.) Gaussen ex Bui for the first time.
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Multi-template molecularly imprinted solid phase extraction not only has the advantages of high selectivity, large adsorption capacity, easy preparation, reuse and low environmental pollution, but also can realize the enrichment and separation of many kinds of compounds. It has attracted wide attention in the extraction and separation of traditional Chinese medicine components. This study summarizes the latest development of multi-template molecularly imprinted solid phase extraction. At the same time, based on the classification of active components of traditional Chinese medicine (flavonoids, alkaloids, phenylpropanol, terpenes, etc.), the latest application of multi-template molecular imprinting solid phase extraction in multi-component separation of traditional Chinese medicine was reviewed, with a view to better application of multi-template molecularly imprinted polymer in active multi-component extraction and separation of traditional Chinese medicine and provide reference for the material basic research of the efficacy of traditional Chinese medicine.
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Oligosaccharides play important roles in many biological processes and have great medicinal potential. The structure-activity study of oligosaccharides is complicated by the diversity and complexity of their structures. This review summarizes the state of oligosaccharide structural analysis in recent years. The ionization methods and dissociation rule of acid oligosaccharides, neutral oligosaccharides and glycopeptides in mass spectrometry are discussed and the methods of extraction and purification of oligosaccharides, the suitable mass spectrometry models for different types of oligosaccharides, and the advantages and disadvantages of different mass spectrometry models are introduced. We believe that this review will be helpful for the further investigation of these important biological substances.
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Based on the previous studies in recent years, this advances made a summary of immunoregulatory effects from Dendrobium officinale. And the research advances on related bioactive compounds of polysaccharides in extraction, separation and purification, structural composition and content determination were systemically reviewed. This paper intended to provide a theoretical basis for reasonable research and exploitation of related health foods of D. Officinale.
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Objective To study the extraction, separation, and in vitro dissolution method of HgS micro & nano-particles from Mongolian medicine Menken Usu. Methods The Soxhlet extraction method was used to investigate the sulfur from Menken Usu effectively, and the optimum time of extraction was determined by investigating the influence of different extraction time on the extraction rate of sulfur in the Menken Usu. Then, the mercuric sulfide particles were separated by differential centrifugation. The mercuric sulfide micro & nano-particles with different particle sizes can be obtained by controlling the concentration of PVP, molar ratio, centrifuge speed, and other factors. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) were used to analyze the morphology and composition of the particles. Using dithizone colorimetric method to determine and compare the dissolution of HgS particles with different sizes, Menken Usu original herbs, and Menken Usu-18 in simulated human gastric and small intestinal. Results The SEM results showed that the obtained six mercuric sulfide particle samples have a uniform size distribution: Uniform size were 2 000-4 000, 800-2 000, 200-800, 80-200, 50-80, and 20-50 nm. The main components in the extracted samples were α-HgS and β-HgS. As the particle size of HgS gradually became smaller, the dissolution of mercury was increased, which indicated that the size of HgS particle was inversely related to the dissolution of mercury. At the same time, the dissolution of mercury is also affected by sulfur, pH, and compounds. Conclusion This is a simple and efficient method for the separation of mercuric sulfide particles, and provides the basis for the pharmacokinetics and pharmacological study of mercuric sulfide nanoparticles with different particle size.
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OBJECTIVE: To study the flavonoid glycosides of Urena lobata. METHODS: Compounds were isolated and purified using various column chromatographies such as D101 macroporous adsorption resin, silica gel, Sephadex LH-20, and prep HPLC. Their structures were identified on the basis of their physicochemical properties and various spectroscopic experiments, including HRESIMS, 1H-NMR, 13C-NMR, HSQC, and HMBC. RESULTS: Ten flavonoid glycosides were obtained from the n-BuOH extract of U. lobata including quercetin-3-O-β-D-glucopyranosyl-(1→2)-β-D-galactopyranoside(1), kaempferol-3-O-β-D-glucopyranosyl-(1→2)-β-D-glucopyranosyl-7-O-α-L-rhamnopyranoside(2), quercetin-3-O-β-D-apiofuranosyl-(1→2)-β-D-glucopyranosyl-7-O-α-L-rhamnopyranoside(3), kaempferol-4'-O-β-D-apiofuranosyl-3-O-β-D-glucopyranosyl-7-O-α-L-rhamnopyranoside(4), kaempferol-3-O-β-D-apiofuranosyl-(1→2)-β-D-glucopyranosyl-7-O-α-L-rhamnopyranoside(5), quercetin-3-O-β-D-glucopyranosyl-7-O-α-L-rhamnopyranoside(6), quercetin-3-O-β-D-glucopyranosyl-(1→2)-β-D-glucopyranoside(7), kaempferol-3-O-α-L-rhamnopyranosyl-(1→6)-β-D-glucopyranosyl-(1→2)-β-D-glucopyranoside(8), kaempferol-3-O-β-D-glucopyranosyl-(1→2)-[α-L-rhamnopyranosyl-(1→6)]-β-D-glucopyranoside(9) and kaempferol-3-O-β-D-glucopyranosyl-(1→2)-β-D-glucopyranoside(10). CONCLUSION: Compounds 1-3 and 6-10 are firstly obtained from U. lobata.
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Separation of active ingredients from Chinese materia medica (CMM) by molecularly imprinted polymers has such advantages as high speed, low cost, being reusable, low pollution, and so on. Because of this reason, the synthesis of molecularly imprinted polymers and its application in separation have drawn more and more attention of researchers in the field of CMM all over the world. Obviously, the core of this research is to explore the relationship between the polymer-structure and separation efficiency. Based on the types of active ingredients of CMM (flavone, alkaloids, phenylpropanoids, terpenoids, etc.), the design principle of molecularly imprinted polymer, its preparation methods and latest application in separation of active ingredients from CMM were introduced. Therefore, this paper can provide a reference for designing new materials with higher selectivity in separation of active ingredients from CMM.
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Punicalin is an important ellagic tannin in Pericarpium Granati with the pharmacological effects such as antioxidation,anti-bacteria,antivirus and anti-inflammation.The studies on Pericarpium Granati at home and abroad were reviewed in the paper,and the extraction,separation,content determination,pharmacological activities and metabolism of punicalin were also summarized to provide theoretical basis for the development and application of punicalin.
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To provide scientific and theoretical basis for the further study and reference for the development and efficient use of the medicinal plants, the extraction and separation technology of Celtis sinensis and its main chemical components and pharmacological effects were summarized. Literatures were reviewed, and the key information was classified and summarized. A large number of flavonoids, triterpenoids, phenols, anthraquinones and amides have been isolated from the plants. Extract of Celtis shows diversed pharmacological activities, such as antioxidant, anti-inflammatory, antibacterial, anti-tumor and so on. Further studies should be carried out on Celtis sinensis, which is abundant in our country and has high medicinal value and broad application prospect, for its better development and utilization.
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Objective: To optimize the extraction process of polysaccharide from Codonopsis pilosula and determine the monosaccharide composition and molecular weight distribution, in order to provide the basis for further separation of C. pilosula polysaccharide. Methods: The content of polysaccharide in C. pilosula was determined by phenol sulfuric acid method, the extraction process of polysaccharide was optimized by orthogonal test. C. pilosula polysaccharides were prepared from crude polysaccharides by deproteinization, decoloration, dialysis, and lyophilization, then monosaccharide composition and mean molecular mass of C. pilosula polysaccharides were analyzed by high performance liquid chromatography (HPLC) and high performance gel permeation chromatography (HPGPC). Results: The extraction temperature was 85 ℃, the extraction time was 1.5 h per time, twice, and solid to liquid ratio was 1:12. Under these conditions, the yield of polysaccharides was 22.57%. The polysaccharides were consisted by glucuronic acid, aminogalactose, xylose, and small quantities of mannose, the average molecular mass was 21 498. Conclusion: This study provides a theoretical basis for the classification and activity of polysaccharide from C. pilosula.
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Objective:To study the extraction and separation of anti-tumor active ingredients from fresh Gekko swinhonis. Meth-ods:The extraction was carried out with ethanol at different concentrations by various methods. The extract was purified by HPLC after deproteinization and degreasing using a repeated freezing and thawing method. MTT was used to detect the antitumor activity of the ex-tract. Results:The A value of extraction process groupⅢwith 85% ethanol ultrasonic extraction was (0. 548 ± 0. 045) with the high-est tumor inhibition rate, and compared with the control group, the difference was significant (P<0. 05). Conclusion:The results of pharmacodynamics show that the optimum extraction technology is ultrasonic extraction with 85% ethanol.
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Aqueous two-phase system (ATPS) is a new liquid-liquid fractionation technique that has been extensively applied in the separation and purification of natural products including proteins, genetic material, bionanoparticles, cells, and secondary metabolites. Advantages of the technique include scale-up potential, continuous operation, ease of process integration, low toxicity, etc. This paper reviewed the applications in separation and purification of the active constituents from Chinese materia medica (CMM) in recent five years, so as to promote the development of separation of the active constituents in CMM.
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Objective: To research the separation, extraction, and quality control of tiliroside from Loropetalum chinense. Methods: The herbs were extracted using ethanol reflux extraction, and then through macroporous resin, depressure silica gel column chromatography, and elution, tiliroside monomer was obtained. Content was determined by the C18 column, mixture of methanol-0.1% phosphoric acid (55:45) as mobile phase at 1.0 mL/min, and UV detection wavelength at 320 nm were used for the determination. Results: Tiliroside can be a good separation of the monomer, with the content of 98%; Tiliroside was better in linear relationship in the range of 0.041-0.513 μg (r = 0.9997). The recovery rate was 100.05%, RSD = 1.50%. Conclusion: Using this method, tiliroside can be better extracted and separated, Meanwhile the determination method is very stable and accurate, and has good repeatability, which can be used for the quality control of tiliroside from L. chinense.
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Compound composition of several natural products including plants,animals,and minerals.In the different needs of Chinese medicine research and application,different extraction and separation methods have been chosen,however,these technologies lacked of scientific and reasonable evaluation criteria because most of these technologies stem from other disciplines,which is the main reason for limited application of the method in Chinese medicine.So the key scientific issue is to establish the quality evaluation system of extraction and separation technology in line with the modern medicine.This article aims to establish the scientific principles of evaluation system for extraction and isolation of Chinese herbal compound.
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Object To extract and separate the chemical constituents from the root of Isatis indigotica Fort (Cruciferae) Methods The root of I. indigotica was percolated with 95% ethyl alcohol, partitioned in solvents of different polarities and finally isolated on silica gel and macroporous resin columns The purified compounds obtained were identified and structurally elucidated by their physicochemical properties and spectral analysis Results Two compounds were obtained and named as isaindigotidione (Ⅰ) and (E)-3-(3′, 5′-dimethoxy-4′-hydroxybenzylidene)-2-indolinone Conclusion The two compounds were new
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Objective To extract and separate crude gingerols and to determine the content of [6]-gingerol in crude gingerols.Methods Crude gingerols were separated from the ginger supercritical-CO2 extracts by silica gel dry column chromatography with solvent system of diethyl ether-n-hexane(7:3).The content of [6]-gingerol in crude gingerols was determined by HPLC.Results [6]-gingerol content in the prepared crude gingerols by silica gel dry column chromatography arrived 52.87 %(m/m).[6]-gingerol had a good linearity in the range of 0.512～ 3.075 ? g,r=0.999 9,and the average recovery was 99.19 %,RSD=1.58 % .Conclusion Silica gel dry column chromatography can be used to quickly,effectively prepare crude gingerols,in which [6]-gingerol content is high,and can supply enough material for further research.The liquid chromatographic analysis of [6]-gingerol is simple,reliable,reproducible and can be used for the quality control of crude gingerols.