OBJECTIVE To optimize an efficient method to synthesize Naftopidil and its chiral enantiomers using silica gel as a catalyst.METHODS 1-naphthyl glycidyl ether and 1-(2-methoxyphenyl)-piperizine were stirring with silica gel(60-100 mesh) at room temperature under nitrogen in solvent-free condition.The reaction conditions were optimized and the chiral enantiomers of Naftopidil were synthesized using these optimum conditions.RESULTS The best result was obtained by using 20% mass percentage of silica gel as the catalyst,with yield up to 87%.Recycling and reusing silica gel for 5 times,we detected no considerable loss of its catalytic ability,with yields all above 70%.When it came to synthesis of chiral Naftopidil enantiomers,the best yield was 77%,the enantiomeric excess of which was as high as 98.2%.CONCLUSION The methods were mild with high yields.Reactants and catalyst were easily separated.Catalyst could be reused for 5 times without apparent degradation.This route suited the basic requirements of green chemistry which had a promising future for industrialization.

Objective To explore conditions for the modification of MAP30 from Semen Momordica Charantiae with polyethylene glycol (PEG) and the method for the purification of PEG-MAP30. Methods To analyze the influence of various conditions on the components of PEG-MAP30 by SDS-PAGE,purify PEG-MAP30 by Sephacryl S-300 HR molecular sieve column chromatography,and detect the modification rate of amino by TNBS under the optimal reaction condition with the reaction of (mPEG)2-NHS and MAP30. Results Temperature 4℃,boric acid-borax buffer with pH 8.5,concentration of MAP30 1 mg/mL,the mass ratio of MAP30 to (mPEG)2-NHS (1∶10),and,5 min for reaction time were selected as the optimal reaction condition. Molecular sieve column showed a good purification effect. The modification rate of amino was 44.9% tested by TNBS under the optimal reaction condition. Conclusion The factors influencing the modification of MAP30 with PEG are determined,and a purification method for PEG-MAP30 is developed.

OBJECTIVE To explore the methods for purification of polysaccharides from Calvatia gigantea,and investigate the characteristics of the polysaccharides.METHODS Polysaccharides form Calvatia gigantea were separated and purified by hot water extraction,ethanol precipitation,and fractionation by ionexchange chromatography on DEAE-sepharose fast flow and Sephacryl S-300 HR chromatography.Sephacryl S-300 HR chromatography,agarose gel electrophoresis,SDS-PAGE,UV spectrum were used to identify the homogenicity of the polysaccharides.The apparent average molecular weight was identified by Sephacryl S-300 HR chromatography.The component of the polysaccharides were identified by GC-MS.The content of uronic acid was identified by carbazole-sulphuric acid analysis.The structural characterizations of the polysaccharides were confirmed by NaIO4 oxidation,Smith degradation and IR.RESULTS Three water-soluble polysaccharides CGP-I,CGP-II and CGP-III were obtained from Calvatia gigantea.Three fractions were shown to be homogeneous by Sephacryl S-300 HR chromatography,agarose gel electrophoresis,SDS-PAGE,and UV spectrum.The apparent average molecular weight of CGP-I,CGP-II and CGP-III were estimated to be 9.12×104 Da,18.6×104 Da and 15.6×104 Da,respectively.The component of polysaccharides:mannose,glucose and galactose were found to be in the molar radio of 1.22:11.28:3.92 in CGP-Ⅰ,1.74:26.45:0.36 in CGP-Ⅱ,1.06:9.9:3.29 in CGP-Ⅲ,and an unknown monosaccharide was found.The content of uronic acid in CGP-Ⅱ,CGP-Ⅲ was 17.2 % and 20.5%,respectively,and there was no uronic acid in CGP-Ⅰ.The results of structural characterization showed that they were all branching chain polysaccharide with more 1→4 linking,fewer 1→6 linking.CGP-Ⅰwas neutral polysaccharide which was mainly composed of pyranose and had both β-and α-epimer,CGP-Ⅱ,CGP-Ⅲ were acidic polysaccharides which were composed of pyranose and had β-epimer.CONCLUSION The preliminary property and structural characterization of the polysaccharides purified from calvatia gigantea were investigated.

To screen the bacteria of degrading the neurotoxin ODAP from 30 kinds of bacteria by microbial fermentation,the consumed amounts of ODAP from Lathyrus sativus extraction as culture medium which contained fixed quantify of ODAP was determined phthaladehyde colorimetric method.The results showed that there were two kinds of bacteria which had the property of consuming obviously ODAP.In addition,the rescarch of this paper included the relativity of the growth and the degradation of ODAP,and the enzyme kinetics of reaction velocity and time.Then it was concluded that it was capable of producing ODAP degrading enzyme by microbial fermentation in culture medium of ODAP.