Physicochemical properties and anti-inflammatory and immunomodulatory effects of Shengfupian polysaccharides / 中国中药杂志

In this study, the crude polysaccharides was extracted from Shengfupian and purified by Sevag deproteinization. Then, the purified neutral polysaccharide fragment was obtained by the DEAE-52 cellulose chromatography column and Sephadex G-100 co-lumn. The structure of polysaccharides was characterized by ultraviolet spectroscopy, infrared spectroscopy, ion chromatography, and gel permeation chromatography. To investigate the anti-inflammatory activity of Shengfupian polysaccharides, LPS was used to induce inflammation in RAW264.7 cells. The expression of the CD86 antibody on surface of M1 cells, the function of macrophages, and the content of NO and IL-6 in the supernatant were examined. An immunodepression model of H22 tumor-bearing mice was established, and the immunomodulatory activity of Shengfupian polysaccharides was evaluated based on the tumor inhibition rate, immune organ index and function, and serum cytokine levels. Research indicated that Shengfupian polysaccharides(80 251 Da) was composed of arabinose, galactose, glucose, and fructose with molar ratio of 0.004∶0.018∶0.913∶0.065. It was smooth and lumpy under the scanning electron microscope. In the concentration range of 25-200 μg·mL~(-1), Shengfupian polysaccharides exhibited little or no toxicity to RAW264.7 cells and could inhibit the polarization of cells to the M1 type and reduce the content of NO and IL-6 in the cell supernatant. It could suppress the phagocytosis of cells at the concentration of 25 μg·mL~(-1), while enhancing the phagocytosis of RAW264.7 cells within the concentration range of 100-200 μg·mL~(-1). The 200 mg·kg~(-1) Shengfupian polysaccharides could alleviate the spleen injury caused by cyclophosphamide, increase the levels of IL-1β and IL-6, and decrease the level of TNF-α in the serum of mice. In conclusion, Shengfupian polysaccharides has anti-inflammatory effect and weak immunomodulatory effect, which may the material basis of Aconm Lateralis Radix Praeparaia for dispelling cold and relieving pain.

Isolation, structural identification of secondary metabolites from Pseudomonas aeruginosa HBD-12 with antibacterial and antitumor activities / 生物工程学报

To screen strains with antibacterial and antitumor activity, pregnenolone was used as the sole carbon source for screening bacteria from soil. Based on bacteriostatic activity assay, Pseudomonas aeruginosa HBD-12 was found to be effectively inhibiting the growth of Escherichia coli, Bacillus thuringiensis, Penicillium digitatum and Penicillium italicum, and its fermentation broth was separated and purified using column chromatography. Then, structure of the obtained monomeric compounds was analyzed by spectrum analysis, and their antitumor activity was measured using HTRF kinase detection kit. The isolated monomeric compounds 1-hydroxy-9,10-phenanthroline and 3-hydroxy-9,10-dihydrophenanthroline had significant antitumor activity. At 20 μg/mL, 1-hydroxy-9,10-phenanthroline and 3-hydroxy-9,10-dihydrophenanthroline inhibited 78.39±2.29% and 60.34±8.35% Aurora kinase A, respectively. Therefore, the secondary metabolites of Pseudomonas aeruginosa HBD-12 have the potential to develop antibacterial and antitumor drugs.

Structural characterization and anti-complement activity of polysaccharides from Glechomae Herba / 中草药

Objective: To isolate and purify the homogeneous polysaccharides from Glechomae Herba through the guidance of anti-complement activity, and study their structures. Methods: Crude polysaccharides from Glechomae Herba were extracted by water extraction and alcohol precipitation, then homogeneous polysaccharides were separated by DEAE-52 and Sephadex G-100 column chromatography. The structures of homogeneous polysaccharides were characterized by HPGPC, IR, GC, methylation and NMR, and their anti-complement activities were also determined. Results: Two homogeneous polysaccharides GLP-1 and GLP-2 were obtained with the molecular weight of 5 370 and 20 040. They were both heteropolysaccharides composed of arabinose and galactose with the ratio of 1:6.3 and 1:4.9, respectively. Conclusion: The structures of GLP-1 and GLP-2 further elucidate the pharmacodynamic basis of their anti-complement activities and provide basis for screening natural complement inhibitors.

Comparative study on different areas of Astragali Radix based on oligosaccharides characteristic map and immunological activity evaluation of partial acid hydrolyzed / 中草药

Objective: The characteristic maps and immunological activities of some acid hydrolysates of polysaccharides from Astragali Radix (APS) from different areas were compared. The quality evaluation method of Astragali Radix with oligosaccharide mixture as quality control index was established. Methods: In this study, the polysaccharides from the traditional Chinese medicine Astragali Radix were used as the research object. Firstly, the optimal partial acid hydrolysis conditions were selected by orthogonal test. The polysaccharide was hydrolyzed into oligosaccharides for analysis. The characteristic map of Astragalus oligosaccharides based on partial acid hydrolysis-hydrophilic interaction chromatography was established. Multivariate statistical analysis was performed on the data by SIMCA software to distinguish Mongolian Astragalus from different areas. The partial acid hydrolysis products of Astragalus polysaccharides were characterized by hydrophilic interaction chromatography and mass spectrometry, and the activity was evaluated by mouse peritoneal macrophage phagocytosis neutral red experiment. Results: The optimal hydrolysis conditions obtained by orthogonal experiment were temperature 90 ℃, trifluoroacetic acid concentration 1 mol/L, hydrolysis time 1 h. Under this condition, Astragalus polysaccharide was hydrolyzed into characteristic oligosaccharide fragments, and the method is reproducible. The characteristic map of Astragalus oligosaccharides based on partial acid hydrolysis-hydrophilic interaction chromatography showed that the maps of the same Astragalus oligosaccharides had good consistency, and the maps of different Astragalus oligosaccharides were quite different. PCA showed that three different kinds of Mongolian Astragalus can be distinguished. It was found by mass spectrometry that the extracted Astragalus polysaccharides were mainly 1→4 linear glucan, and gluco-oligosac-charides with the degrees of polymerization 3—8 were obtained after partial acid hydrolysis. The partial acid hydrolysate of the wild Astragalus polysaccharides from Shanxi Hunyuan had higher ability to enhance the phagocytic activity of macrophages than the transplanted Astragalus and higher than the unhydrolyzed total astragalus polysaccharide. Conclusion: This study showed that the characteristics of Astragalus polysaccharides based on partial acid hydrolysis-hydrophilic interaction chromatography and the effects on cellular immune function can be used to evaluate the quality of Astragali Radix in different habitats and different planting methods, and it is also an important supplement to the quality evaluation method of Astragali Radix. At the same time, it has a certain exemplary role in the characterization of other Chinese materia medica polysaccharides.

Chemical Structure and Morphological Features of A Polysaccharide BHP-1 Purified from Bulbs of Lilium davidii var. unicolor / 中国实验方剂学杂志

Objective::To study the chemical structure and morphological features of a polysaccharide BHP-1 isolated and purified from the bulbs of Lilium davidii var. unicolor. Method::Thermogravimetry (TG) and scanning electron microscopy (SEC) was used to determine the thermal characteristics and the surface morphology changes of the polysaccharide BHP-1, respectively. The chemical structure of BHP-1 was analyzed by gas chromatography-mass spectrometer (GC-MS), partial acid hydrolysis, sodium periodate oxidation-Smith degradation and nuclear magnetic resonance (NMR). Result::The results showed that the backbone of the polysaccharide BHP-1 mainly contained α-(1→4)-linked D-glucopyranosyl and β-(1→4)-linked D-mannopyanosyl, and the branches were probably linked at the O-2 and/or O-3 of the mannosyl and glucosyl residues, with T-α-D-glucopyranosyl as a terminal structure. It was a natural mannoglucose containing a small amount of O-acetyl group. BHP-1 began to degrade at 220 °C, and the degradation ended at 520 ℃, indicating a good thermal stability, smooth surface and a large number of depressions. The depressions were formed by closely interlaced and sunken sheet layers with irregular holes. Conclusion::BHP-1 was a natural mannoglucose with a good thermal stability, smooth surface, a large number of depressions and irregular holes, and contained a small amount of O-acetyl group. Its chemical structure was reported for the first time.

Structure and application of Ganoderma polysaccharide peptide GL-PPSQ2 / 中草药

Objective To study the structure of active polysaccharide peptide purified from Ganoderma lucidum aqueous extract, and used as a reference substance for the determination of polysaccharide peptide content in G. lucidum products. Methods GL-PPSQ2 was obtained by hot water extraction, separation and purification with membrane ultrafiltration and gel-filtration chromatography. The physicochemical determination and spectral date were used for structural identification. The content of polysaccharide peptide was detected by HPLC with UV detector, water was used as mobile phase and the flow rate was 1 mL/min. Results GL-PPSQ2 was a pure polysaccharide peptide with purity above 97%, molecular weight of 5.0 × 104, polysaccharide content of 87.17%, and yield of 0.49%. The monosaccharides composition analysis showed that GL-PPSQ2 was glucose-based polysaccharide with a small amount of mannose, which contained 16 kinds of amino acids with the total amount of amino acids of 5.04%. Based on the methylation analysis, 1D and 2D NMR spectroscopy, the repeating unit of GL-PPSQ2 was composed of →3)-β-D-Glcp-(1→backbone, with four repeating units connected a long chain branch at O-6 which was composed of α-D-Glcp-(1→, →4,6)-β-D-Glcp-(1→, →4)- β-D-Glcp-(1→ and →6)-β-D-Glcp-(1→ in sequence. Conclusion The active polysaccharide peptide was isolated and purified by membrane technology and gel chromatography. The method was simple and rapid, which provided a scientific basis for the quality control of polysaccharide peptide in G. lucidum extract and its products.

Isolation, purification and structural characterization of Bletilla striata polysaccharides and its antitumor activity / 中草药

Objective: Bletilla striata polysaccharide (BSP-1) extracted from the stem tubers of B. striata was purified to study the structural properties and antitumor activity. Methods: The crude polysaccharide was fractionated by DEAE-cellulose column chromatography, and three fractions were obtained including BP-1, BP-2, and BP-3, respectively, BP-1 was further purified by SephadexG-200 column chromatography, and a sub-fraction named BSP-1 was obtained. Subsequently, HPGPC, IR spectroscopy, gas chromatography (GC), GC coupled to mass spectrometry (GC-MS) and methylation analysis, and 1H- and 13C-NMR were employed to characterize the structural properties of the polysaccharide fractions. Moreover, the anticancer activity was investigated in vivo. Results: The results showed that the molecular weight of BSP-1 were 4.72 × 105. BSP-1 was consisted of mannose (Man) and glucose (Glc) residues. The backbone of BSP-1 was composed of β-1,4-linked Man and Glc residues at the end with a molar ratio of 8:1. BSP-1 could inhibit the tumor proliferation of HepG2-bearing mice. The tumor weight of mice was significantly inhibited by BSP-1 with inhibitory rate of 66.42%. Conclusion: Structural characterization of BSP-1 provides the significant reference for the further development and elucidation of polysaccharides from B. striata as new drugs.

Structural characterization of polysaccharide from Polygonum multiflorum and its immunomodulatory activity / 中草药

Objective: To extract and separate a polysaccharide from Polygonum multiflorum, characterize its structural features and study its immunomodulatory activity. Methods The polysaccharide from P. multiflorum (PMT) was isolated and purified by water extraction and ethanol precipitation following Q-Sepharose Fast Flow ion exchange chromatography column. Molecular weight of PMT was determined by high performance gel permeation chromatography-multiple angle laser light scattering (HPGPC-MALLS), and monosaccharide composition was analyzed by HPLC with PMP (1-phenyl-3-methyl-5-pyrazolone) pre-column derivatization, respectively. The structure of PMT was characterized by proton nuclear magnetic resonance spectrum (2D-NMR). The immunomodulatory activities were tested by MTT, neutral red colorimetric assay and Griess method. Results: PMT was a kind of α-1,4-glucan, and its molecular mass was 3.96 × 105. PMT promoted the proliferation and phagocytosis of RAW 264.7 cells, and significantly induced the increase of NO production in a dose-dependent manner. Conclusion: The polysaccharide from P. multiflorum is a linear α-1,4-glucan with potent immunomodulatory activity, which would be potentially developed as an effective drug.

Fractionation, structural characterization, and immunomodulatory activity of polysaccharide isolated from Ganoderma lucidum / 中草药

Objective To extract, separate, and purify polysaccharide from Ganoderma lucidum with alkali from the residue after water extraction, characterize the basic physicochemical properties and structural features in detail, and study the immunomodulatory activity in vitro. Methods The polysaccharide LZJ-015 was isolated and purified from the dry fruiting bodies of G. lucidum by alkaline extraction and ethanol precipitation following Q-Sepharose Fast Flow ion exchange chromatography column. Monosaccharide composition and molecular weight of LZJ-0.15 was analyzed by high performance liquid chromatography (HPLC) with PMP precolumn derivatization and high performance gel permeation chromatography-multiple angle laser (HPGPC-MALLS), respectively. The detailed structure of polysaccharide LZJ-0.15 was characterized by 1H-NMR, 13C-NMR, 1H-1H COSY, and 1H-13C HSQC spectrum. The immunomodulatory activity of G. lucidum polysaccharide was test by RAW264.7 cells phagocytose neutral red experiment. Results The molecular weight, molecular radius, and Mw/Mn of LZJ-0.15 were determined to be 24 700, 46.6 nm, and 1.019, respectively. The monosaccharide composition was confirmed to be mainly composed of glucose (92.3%). LZJ-0.15 was →3) Glc (β1→and→6) Glc (β1→linked glucan indicated by NMR spectrum. Moreover, G. lucidum polysaccharide exhibited good immunomodulatory activity in our study. Conclusion G. lucidum polysaccharide LZJ-0.15 from alkaline extraction showed better immune activity than the polysaccharide extracted from water, which would be potentially developed as an effective immunomodulatory agent.

Structural confirmation of sulconazole sulfoxide as the primary degradation product of sulconazole nitrate / 药物分析学报

Sulconazole has been reported to degrade into sulconazole sulfoxide via sulfur oxidation; however, structural characterization data was lacking and the potential formation of an N-oxide or sulfone could not be excluded. To clarify the degradation pathways and incorporate the impurity profile of sulconazole into the United States Pharmacopeia–National Formulary (USP–NF) monographs, a multifaceted approach was utilized to confirm the identity of the degradant. The approach combines stress testing of sulco-nazole nitrate, chemical synthesis of the degradant via a hydrogen peroxide-mediated oxidation reaction, semi-preparative HPLC purification, and structural elucidation by LC―MS/MS and NMR spectroscopy. Structural determination was primarily based on the comparison of spectroscopic data of sulconazole and the oxidative degradant. The mass spectrometric data have revealed a McLafferty-type rearrange-ment as the characteristic fragmentation pathway for alkyl sulfoxides with aβ-hydrogen atom, and was used to distinguish the sulfoxide from N-oxide or sulfone derivatives. Moreover, the generated sulco-nazole sulfoxide was utilized as reference material for compendial procedure development and valida-tion, which provides support for USP monograph modernization.

Polysaccharide rich fractions from barks of Ximenia americana inhibit peripheral inflammatory nociception in mice Antinociceptive effect of Ximenia americana polysaccharide rich fractions

Abstract Ximenia americana L., Olacaceae, barks are utilized in folk medicine as analgesic and anti-inflammatory. The objective was to evaluate the toxicity and antinociceptive effect of polysaccharides rich fractions from X. americana barks. The fractions were obtained by extraction with NaOH, followed by precipitation with ethanol and fractionation by ion exchange chromatography. They were administered i.v. or p.o. before nociception tests (writhing, formalin, carragenan-induced hypernociception, hot plate), or during 14 days for toxicity assay. The total polysaccharides fraction (TPL-Xa: 8.1% yield) presented 43% carbohydrate (21% uronic acid) and resulted in two main fractions after chromatography (FI: 12%, FII: 22% yield). FII showed better homogeneity/purity, content of 44% carbohydrate, including 39% uronic acid, arabinose and galactose as major monosaccharides, and infrared spectra with peaks in carbohydrate range for COO- groups of uronic acid. TPL-Xa (10 mg/kg) and FII (0.1 and 1 mg/kg) presented inhibitory effect in behavior tests that evaluate nociception induced by chemical and mechanical, but not thermal stimuli. TPL-Xa did not alter parameters of systemic toxicity. In conclusion, polysaccharides rich fractions of X. americana barks inhibit peripheral inflammatory nociception, being well tolerated by animals.

Characterization and bioactivities of a novel polysaccharide obtained from Gracilariopsis lemaneiformis

ABSTRACT Gracilariopsis lemaneiformis is a type of red alga that contains seaweed polysaccharide agar. In this study, a novel non-agar seaweed polysaccharide fraction named GCP (short of crude polysaccharide obtained from Gracilariopsis lemaneiformis) was isolated from Gracilariopsis lemaneiformis. Structural analysis showed that GCP shows triple helical chain conformation when dissolved in water and has many branches and long side chains. Also, 1→3 linkage is the major linkage and the sugar structures are galactopyranose configurations linked by β-type glycosidic linkages. Two macromolecular substance fractions (GCP-1 and GCP-2) were purified by DEAE Sepharose Fast Flow column chromatography. Moreover, a splenocyte damage assay and splenocyte proliferation assay were used to analyse the bioactivities of GCP, GCP-1 and GCP-2. It was demonstrated that polysaccharides could protect splenocyte damaged by H2O2; GCP-2 shows a greatest protection rate, that is, 92.8%, which significantly enhanced the splenocyte proliferation, and GCP showed the highest proliferation rate, 9.30%. The results suggested that this type of novel non-agar polysaccharide displayed remarkable antioxidant and immunomodulatory activities and early alkali treatment could decrease the activities. It may represent a potential material for health food and clinical medicines.

Caracterização do estado sólido de ganciclovir / Solid state characterization of ganciclovir

O presente trabalho teve como objetivo o estudo do estado sólido do ganciclovir (GCV) e suas diferentes formas polimórficas. O GCV é um fármaco antiviral útil no tratamento de infecções por citomegalovírus (CMV). Embora seja um fármaco amplamente usado, poucos estudos têm sido realizados sobre seu estado sólido. Atualmente, o GCV é conhecido por apresentar quatro formas cristalinas, duas anidras (Forma I e II) e duas hidratas (III e IV). Neste trabalho, nós reportamos a solução da estrutura cristalográfica da Forma I do GCV, que foi encontrado durante o screening de cristalização do fármaco, em que nove ensaios de cristalização (GCV-1, GCV-A, GCV-B, GCV-C, GCV-D, GCV-E, GCV-F, GCV-G e GCV-H) foram realizados e os materiais resultantes foram caracterizados por Difratometria de raios X (DRX), análise térmica (DTA/TG) e Hot Stage Microscopy. De todas as cristalizações realizadas foram obtidas quatro formas sólidas, denominadas como Forma I (GCV-1, GCV-B e GCV-H), Forma III (GCV-C, GCV-D, GCV-F e GCV-G), Forma IV (GCV-A) e Forma V (GCV-E). Esta última está sendo descrita pela primeira vez na literatura e indica a presença de outra forma hidratada de GCV. As Formas I, III e IV corresponderam a forma anidra e as duas formas hidratadas do fármaco, respectivamente. Além disso, foi evidenciado por experimentos de conversão de slurry e análise térmica que o cristalizado de GCV-1 (Forma I) foi o mais estável entre os materiais obtidos, e este deu origem ao monocristal da Forma I de GCV, estrutura cristalina anidra do fármaco. Neste trabalho, pela primeira vez, a estrutura cristalina deste composto foi definida por cristalografia de raios X de monocristal. A análise estrutural mostrou que a Forma I do fármaco cristaliza no grupo espacial monoclínico P21/c e está composta por quatro moléculas de GCV na sua unidade assimétrica. Cada molécula está unida intermolecularmente por ligações de hidrogênio, que dão lugar à formação de cadeias infinitas e estas por sua vez se arranjam de maneira a formar uma estrutura tridimensional.

This presented work aims to study the solid state of ganciclovir (GCV) and its different polymorphic forms. GCV is an antiviral drug useful in the treatment of cytomegalovirus (CMV) infections. Although it is a widely-used drug, few studies have been conducted on its solid state. Currently, GCV is known to have four crystalline forms, two anhydrous (Form I and II) and two hydrates (III and IV). In this investigation, we report a successful preparation of GCV Form I and its crystallographic structure, which was found during the crystallization of the drug, in which nine crystallization tests (GCV-1, GCV-A, GCV-B, GCV- D, GCV-E, GCV-F, GCV-G and GCV-H) were performed and the resulting materials were characterized by X-ray diffractometry (XRD), thermal analysis (DTA/TG) and Hot Stage Microscopy. Of all the crystallizations performed, four solid forms were obtained, denoted as Form I (GCV-1, GCV-B and GCV- H), Form III (GCV-C, GCV-D, GCV-F and GCV-G), Form IV (GCV-A) and Form V (GCV-E). The latter is being described for the first time in the literature and indicates the presence of another hydrated form of GCV. Forms I, III and IV corresponded to the anhydrous form and the two hydrated forms of the drug, respectively. In addition, it was evident by both the slurry conversion and the thermal analysis methods that the GCV-1 crystallized (Form I) was indeed the most stable amongst the materials obtained. This gave rise to GCV Form I monocrystal, anhydrous crystalline structure of the drug. The compound was characterized by monocrystal X-ray crystallography. The structural analysis showed that Form I of the drug crystallized in the monoclinic system space group P21/c is composed of four molecules of GCV in its asymmetric unit. Each molecule is linked intermolecularly by hydrogen bonds, which give rise to the formation of infinite chains arranged in a way that form a three-dimensional structure.

Structural characterization of Sophora alopecuroides polysaccarides and study on its antitumor activity of CT26 / 中草药

Objective: To study the structure of Sophora alopecuroides polysaccarides (SAP) and its antitumor activity on CT26 transplanted tumor in mice. Methods: The structure was characterized by high-performance gel permeation chromatography (HPGPC), gas chromatography-mass spectrometer (GC-MS), infrared spectroscopy (IR), and nuclear magnetic resonance spectroscopy (NMR). And then the anticancer activity of CT26-bearing mice was investigated in vivo. Results: The results showed that SAP was consisted of D-mannopyranose and D-galactopyranose residues. The main chain of the galactomannan comprises β-(1,4)-linked D-mannopyranose residues, with branches of galactose, linked to the carbohydrate core through α-D-Gal (1,6) linkage. SAP could inhibit the tumor proliferation of CT26-bearing mice in a dose-dependent manner with inhibitory rate of 44.03% at high dose. Conclusion: Structure determination of SAP provides the theoretical basis for structure-activity relationship study. And it is expected to be further developed as a new antitumor drug with high efficiency and low toxicity.

Isolation, identification and structural characterization of secondary metabolites from amarine sponge-derived rare actinobacterium Dermacoccus sp. X4 / 生物工程学报

We isolated and identified the symbiotic and adnascent microorganisms from an unidentified sponge collected from 10-meter-deep seawater of the Paracel Islands in China. A total of 16 strains were obtained and identified. Through bacteriostatic activity assay, one of the strains, Dermacoccus sp. X4, was found to effectively inhibit the growth of Staphylococcus aureus. Subsequently, its secondary metabolites were purified by silica gel partition, octadecylsilane (ODS) reverse phase, Sephadex™LH-20 size exclusion, and C18 reverse phase chromatography. Using liquid chromatography, mass spectrometry, and nuclear magnetic resonance, three of the purified compounds were structurally characterized to be one 3-(4-hydroxybenzyl) hexahydropyrrolo [1,2-a]pyrazine-1,4-dione and two indole acid glycerides. This is the first report about indole acid glyceride isolated from microbial secondary metabolites, enriching marine drug candidate resources.

Preparation and structural characterization of TiO2 nanotube arrays on surface of orthopaedic titanium plate / 国际生物医学工程杂志

Objective The TiO2 nanotube arrays,fabricated on the surface of orthopedics,was characterized,to provide carrier for orthopedics plant surface modification or coating,and seek a new way for the prevention and treatment of orthopedics plant infection.Methods By adjusting certain parameters,TiO2 nanotube arrays were fabricated on orthopedic titanium plate surface using the method of anodic oxidation,with glycerol system as electrolyte,orthopedics titanium plate as anode,and platinum electrode as cathode.TiO2 nanotube arrays were characterized.The element composition of TiO2 nanotube arrays was analyzed by X-ray photoelectron spectroscopy (XPS),and the morphological changes of TiO2 nanotube arrays was observed at high temperature (300 ℃) by X-ray diffractomer (XRD).Results With glycerol system as electrolyte,TiO2 nanotube array with diameter of about 100 to 200 nm and the length less than 3μm can be fabricated on orthopedic titanium plate surface using anodic oxidation of 24 h.The surface of orthopedic titanium plate was changed from silver white to deep blue in the macroscopic view.The TiO2 nanotube array on orthopedics titanium plate surface was mainly composed of Ti element (75.88％),O element (20.16％),and F element (3.96％) by XPS analysis.TiO2 nanotube arrays morphology was stable when it was heated to 300 ℃ by muffle furnace.Conclusions The method of anodic oxidation can be applied to manufacture TiO2 nanotubes array on titanium plate surface.The array with stable morphology,the inner hollow shape,the bottom sealing,and a large specific surface area,can withstand high temperature,which can provide carrier for orthopedics plant surface modification or coating.

Structural characterization of Guiqi polysaccharides AAP-2A / 中草药

Objective: To isolate the Guiqi (Angelicae Sinensis Radix and Astragali Radix) polysaccharides (AAP) and study the structural characterization of AAP-2A. Methods: Hot water extracting and ethanol precipitating method was employed to isolate the AAP. A new fraction (AAP-2A) of AAP was obtained after AAP was purified by deproteination, gel chromatography on DEAE-52 cellulose, gel chromatography on Sephadex G-100, and other means. Sugar content of AAP-2A was determined using phenol sulfuric acid method. Chromatography techniques were used to determine the ultraviolet properties, infrared properties, relative molecular weight, absolute molecular weight, molecular conformation and molecular weight distribution, and monosaccharide composition with the molar ratio of AAP-2A. The connection, main chain and branched-chain structures, and the condition of branching point were studied by methylation and NMR methods. Results: The total sugar content of AAP-2A, which was absent of proteins and nucleic acids, was 98.98%. Infrared spectroscopy showed that AAP-2A had the typical signals of polysaccharides. The relative and absolute molecular weights of AAP-2A were above 6.68 × 105 and 2.252 × 106; AAP-2A was a neutral sugar and composed of rhamnose (Rha), galactose (Gal), arabinose (Ara), and glucose (Glc) with a molar ratio of 1 : 2.13 : 3.22 : 6.18. AAP-2A proved to be a heteropolysaccharide, with 1, 3-α-L-Rha, 1,3-β-D-Gal, 1,3-, 1,5-, and 1,3,5-α-L-Ara, 1,4- and 1,4,6-α-D-Glc residues in backbone and 1-α-D-Glcp residues in branches. Conclusion: AAP-2A is a new neutral heteropolysaccharide from Guiqi polysaccharides with a highly branched conformation.

Structural characterization of C-glycosyl flavonoids in Scutellaria baicalensis and differentiation of isomers by UPLC/LTQ-Orbitrap-MS / 中草药

Objective: An UPLC-LTQ-Orbitrap-MS spectrometry method has been developed for the efficient separation and detection of C-glycosyl flavonoids in the extract of Scutellaria baicalensis differentiation of isomers. Methods: Data were acquired by Orbitrap. MS2, MS3, and MS4 data were triggered by data-dependent acquisition mode. Isomers of C-glycosyl flavonoids were distinguished by a comparison study of mass distribution. Results: A total of 19 compounds were identified as C-glycosyl flavonoids, and several isomers were successfully discriminated. Conclusion: This method is proved to be powerful for the identification of C-glycosyl flavonoids and provides the important complementary information for other flavonoid analysis.

Chemical constituents of roots of salvia plebeia / 中国药学杂志

OBJECTIVE: To study the chemical constituents of the roots of Salvia plebeia R.Br.

Chemical constituents from the stem of Brosimum potabile (Moraceae) / Constituintes químicos do cerne de Brosimum potabile (Moraceae)

Three coumarins, 5-methoxypsoralene, xanthyletin, and (-)-marmesin, have been isolated from the ethanolic extract of the stem of the Amazonian plant Brosimum potabile. The structures were determined on the basis of NMR analyses and by comparison with spectroscopic data in the literature. The analysis of the hexane fractions by GC-MS in EIMS mode suggested the presence of (1-methylpentyl)-benzene; α,α-dimethyl-4-(1-methylethyl)-benzenemethanol; 1-methyl-3,5-bis(1-methylethyl)-benzene; urs-12-ene; chola-5,22-dien-3ß-ol; cholesta-4,6-dien-3ß-ol; sitosteryl 9(Z)-octadecenoate; cholesta-5,22-dien-3ß-ol; cholesta-4,6,22-trien-3-one; and cholesta-4,22-dien-3-one. NMR data of other hexane fractions indicated the presence of 3ß-acetoxy-lup-12,20(29)-diene; 3ß-acetoxy-olean-12-ene; 3ß-acetoxy-urs-12-ene; and adian-5-ene. All these compounds are first described in B. potabile.

Três cumarinas, 5-metoxipsoraleno, xantiletina e (-)-marmesina, foram isoladas no extrato etanólico do cerne da planta amazônica Brosimum potabile. Suas estruturas foram determinadas a partir das análises por RMN e por comparação com dados espectroscópicos da literatura. As análises das frações hexânicas por CG/EM sugeriram a presença de (1-metilpentil)-benzeno; α,α-dimetil-4-(1-metiletil)-benzenometanol; 1-metil-3,5-bis(1-metiletil)-benzeno; urs-12-eno; cola-5,22-dien-3ß-ol; colesta-4,6-dien-3ß-ol; (9Z)-octadecenoato de sitosterila; colesta-5,22-dien-3ß-ol; colesta-4,6,22-trien-3-ona e colesta-4,22-dien-3-ona. Dados de RMN de outras frações hexânicas indicaram a presença de 3ß-acetóxi-lup-12,20(29)-dieno; 3ß-acetóxi-olean-12-eno; 3ß-acetóxi-urs-12-eno e adian-5-eno. Todos esses compostos foram identificados pela primeira vez em B. potabile.