Synthesis of dihalogenated coumarin derivatives for monitoring acid phosphatase activity

Aim To synthetize 6-chloro-8-fluoro-4-methylumbelliferone phosphate(CF-MUP) and utilize it to analyze acid phosphatase activity.Method CF-MUP obtained by phosphorylation of CFMU(6-chloro-8-fluoro-4-methylumbelliferone) which was prepared by Pechmann reaction between 4 and ethyl acetoacetate in the presence of methanesulfonic acid.And then,the utility of CF-MUP as a substrate for acid phosphatase was compared with MUP(4-methylumbelliferone phosphate).Results The new coumarin phosphate,CF-MUP,demonstrated much higher sensitivity and was more robust for detecting the activity of acid phosphatase than MUP in the physiological pH range.Conclusion This new fluorescence dye,CF-MUP,is a convenient tool for the continuous assay of acid phosphatases with a wide range of pH.

Adsorption of Cr(Ⅵ) in wastewater using magnetic multi-wall carbon nanotubes

Magnetic multi-wall carbon nanotubes were prepared with wet chemical treatments and characterized by a transmission electron microscope （TEM） and X-ray diffraction （XRD）. They were used as adsorbents for the removal of Cr（VI） in aqueous solutions. The effects of adsorbent dosage, the concentration of Cr（VI） in aqueous solution, temperature, and pH value on the removal efficiency were studied. Results showed that the adsorption capacity of the magnetic multi-wall carbon nanotubes increased with the initial Cr（VI） concentration, but decreased with the increase of adsorbent dosage. The adsorption amount increased with contact time. The adsorption kinetics were best represented by the pseudo second-order kinetic model, and the adsorption isotherms indicated that the Langmuir model better reflected the adsorption process. The ob- tained calculation results for the Gibbs free energy revealed that the adsorption was a spontaneous and endothermic process. The enthalpy deviation was 3.835 kJ.mol 1. The magnetic multi-wall carbon nanotubes showed significant potential for application in adsorption of heavy metal ions.

Synthesis and characterization of a new water-soluble sodium 5,7,4'-trihydroxyflavone-6,3'-disulfonate

Aim To synthesize a new water-soluble Na 2(C15H8O5)(SO3) 2 and determine its structure.Method The new water-soluble apigenin sulfonated derivative was synthesized by sulfonation with concentrated sulfuric acid at 40℃for half an hour and the products were obtained in ethanol-water(V∶V =1∶1).The structure of the product was identified by IR,NMR spectrum and elemental analysis.Results and Conclusion After highly selective introduced two - SO 3 groups at C3′and C6of the substrate,the new water-soluble apigenin sulfonated derivative,sodium 5,7,4 '-trihydroxyflavone-6,3′-sulfonate was obtained in good yield(78%) at moderate conditions.This method is an ideal synthesis way because of its simple operation,mild reaction conditions,high selectivity,easy separation of the product and higher yield.

Study on the insecticidal activities of the extracts from four plants under orthogonal test

Aim To prepare dry powder insecticide by mixing the plant samples of Aconitum ochranthum Mey.,Aconitum hemsleyanum Pritz.and Dictamnus dasycarpus Turcz.Method The dosage ratios of the break stocks from the plants mentioned above are installed as four factors,and three levels are selected for every factor.The test is actualized according to L 9(3 4) orthogonal array.Results An optimized recipe A 3 B 3 C 3 D 1 has been obtained after considering multifarious factors such as the resources of these plants and the water-solubility of samples.Conclusion The dry powder insecticide prepared by mixing the plant samples mentioned above as 1∶1∶1mass ratio revealed that insecticidal activities for cickets,grasshopper,aphid,and 3rd instar Mythimna separata walker are significant,respectively.

Structure modification of unsaturated natural products:The epoxidation of carbon-carbon double bonds in some natural products with hydrogen peroxide catalyzed by iodine

Aim To afford an environmentally benign catalytic epoxidation of carbon-carbon double bonds in organic substrates using hydrogen peroxide as an oxidant and iodine as a catalyst.Method The effects of different factors on the epoxidation of three unsaturated natural products were investigated by orthogonal design.Results The experimental results show that three unsaturated natural products are oxidized to the corresponding epoxides with hydrogen peroxide in the presence of 10%(mol/mol) of iodine at room temperature in high yields.Conclusion Iodine was found to be an efficient catalyst for the epoxidation of carbon-carbon double bonds in some unsaturated natural products with hydrogen peroxide at room temperature.

Thermodynamic properties of three alkaloids in normal saline

Aim To provide a potent reference for the clinical application of these alkaloids.Method The enthalpy of dissolution for these alkaloids in normal saline are measured using a RD4962000Calvet Microcalorimeter at 36.5℃under atmospheric pressure.Results The differential enthalpy(Δ dif H m) and molar enthalpy(Δ sol H m) were determined for these alkaloids in normal saline.Conclusion On the basis of these experimental data and calculated results,the kinetic equation,half-life,Δ sol H m,Δ sol G m andΔ sol S m of the dissolution process were also obtained.

Several oxygenated monoterpenes from petals of Rosa damascena

Aim To discover the oxygenated monoterpenes that play a critical role in the biosynthetic pathway of monoterpene in Rosa damascene.Method Several kinds of isolation techniques such as liquid-liquid partition,silica column chromatography,thin layer chromatography and high performance liquid chromatography were used to separate the compounds and several identification techniques such as GC-MS and 1H-NMR were used to determine the structure of the isolated compounds.Results Three oxidized acyclic monoterpenes were obtained.They are 8-hydroxygeraniol,8-hydroxynerol and 8-hydroxylinalool.Conclusion The compounds are the important materials of pharmaceutical,cosmetic and food industries.The work has not only provided a new method for the determination of the main aromatic components of Rosa damascena,but also built up an important foundation for the study of biosynthesis of monoterpenoids in the plant.

Immobilized-metal affinity chromatography adsorbent with paramagnetism and its application in purification of the proteins in the natural products

Aim To investigate a new method for synthesis of an Immobilized-Metal Affinity Chromatography(IMAC) adsorbent with superparamagnetism(Fe3O4/SiO2-GPTMS-Asp-Co).Method The magnetic microspheres were synthesized in situ modification and the transmission electron microscope,field emission scanning electron microscopy,X-ray diffractometer,energy spectrometer and vibrating sample magnetometer were used to characterize the appearance,particle size distribution,phase composition,chemical constituents and magnetic properties of silica magnetic microspheres(MMS).Results The silica MMS prepared by reverse microemulsions exhibit a superior core-shell structure.The size distribution of the microspheres varies from between 100 nm to 200 nm and the main phase of microspheres is amorphous SiO2 and spinel Fe3O4.The microspheres retain superparamagnetism and can be used as biomaterials.Conclusion The result indicates that the IMAC adsorbent we prepared has outstanding advantages in the separation of the natural products proteins from the crude bacterial lysate,such as simple operation,high selectivity and capacity.

Traditional Chinese medicine mask for freckles-removal and its preparation

Aim To investigate Traditional Chinese medicine(TMC) mask for freckles-removal because failed facial expression of qi(气) and blood due to their stasis and transport stagnancy is the key factor causing freckles.Method Traditional Chinese medicine is used to remove freckles.TMC mask,which contains Angelica sinensis,Angelica dahurica,Ampelopsis japonica,Bletilla striata,Ligusticum chuanxiongand Asarum sieboldii Miq 100g respectively,is the most respected in facial skin cosmetology in recent years.Results TCM facial mask is used to remove age spots and freckles.They generally help to make the skin smooth and firm and also help in curing freckles gradually.Conclusion The specific active ingredients along with breakthrough of skin absorption barrier are the keys for its effectiveness.

Alkaloidal compounds and bioactivities of three medicinal plants of Menispermaceaefamily in Qinling Montain

Aim To find the original active compounds from three medicinal plants of Menispermaceae family in Qinling Montain,Shaanxi,China.Method Several kinds of isolation techniques such as liquid-liquid partition,column chromatography,thin layer chromatography and sephadex LH-20 gel chromatography are used to separate the compounds and all kinds of identification techniques such as mass,high resolution mass,1H-NMR,13C-NMR,all kinds of 2D-NMR,CD spectra and X-ray diffraction analysis are used to determine the structure of the isolated compounds;several enzymes linked immunosorbent assay are used to test the biological activities of some isolated compounds.Results 30 alkaloids were isolated and identified from Sinomenium acutum of which 8 are new compounds;nine alkaloids were isolated and identified from Menispermum dauricum of which 6 are new compounds;six alkaloids were isolated and identified from Stephania epigaea.Among all the identified alkaloids,six compounds show protective effects against hydrogen peroxide induced cell injury;eight compounds show weak or strong cytotoxicity activity;one compound shows neuroprotective effect against hydrogen peroxide and.β-amyloid25-35-induced oxidative injury.Conclusion These three plants of Menispermaceae family may be considered as the potential drugs for Alzheimer's disease therapy and anticancer agents.