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    30 August 2007, Volume 27 Issue 04 Previous Issue    Next Issue
    研究报告
    Studies on Synthesis and Repellent Activity of 8-Hydroxylcarveol and Its Derivatives
    WANG Zong-de;CHEN Jin-zhu;SONG Zhan-qian;JIANG Zhi-kuan;HAN Zhao-jiu;CHEN Chao
    2007, 27 (04):  1-6. 
    Abstract ( 622 )   PDF (1068KB) ( 660 )   Save
    8-Hydroxylcarveol(3) and its ester derivatives were synthesized from α-pinene(1), and their structures had been identified by IR, MS, 1H NMR and 13C NMR analysis. The repellent activity against mosquito (Aedes albopictus) of the 4 compounds has been determined by the methods of GB 17322.10-1998. The results are as follows: compound (3) has no repellent against mosquito. On the other hand, it has been reported that compounds having structure simlar to 8-hydroxylcarveol have mosquito-repellent activity, such as p-menthendiol, etc. Perhaps the position of polar functional groups and chiral C atoms are important factors for mosquito-repellent activity. 8-Hydroxylcarveol propionate (6) has no mosquito-repellent activity mosquito, perhaps its carbonyl part is too large. There is few report of propionate used as terpenoid repellent currently. 8-Hydroxylcarveol acetate(5) has some repellent activity against mosquito, when its mass fraction is 20%, which can exhibit repelling time close to 4 h. 8-Hydroxylcarveol formate (4) has the longest repelling time of upto 7-8 h against mosquito, when its mass fraction is 20%, which is similar to the repellent activity of N,N-diethyl-m-toluamide (DETA).
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    Study on Enzymatic Hydrolysis of Corncob for Ethanol Production
    ZHAO Jing;CHEN Ming;ZHANG Jing-fang;XIA Li-ming
    2007, 27 (04):  7-10. 
    Abstract ( 671 )   PDF (823KB) ( 722 )   Save
    Enzymatic hydrolysis of corncob for ethanol fermentation from cellulosic hydrolysate was investigated. Corncob pretreated with dilute sulfuric acid was hydrolyzed by the cellulase from Trichoderma reesei ZU-02 at 50℃, pH value 4.8, and the hydrolysis yield was only 67.5% due to poor cellobiase activity in T. reesei ZU-02 cellulase. Addition of cellobiase from Aspergillus niger ZU-07 greatly reduced the inhibitory effect caused by cellobiose, and the hydrolysis yield was improved to 83.9% with cellobiase dosage of 6.5 CBIU/g substrate. A hydrolysis process using batch-wise feed was carried out to get a final substrate concentration of 200 g/L and the hydrolysis yield reached 80.1% after 60 h reaction. Furthermore, ethanol fermentation of cellulosic hydrolysate containing 95.3 g/L glucose was performed at 38℃ using a thermotolerant strain Saccharomyces cerevisiae HTR-11,45.7 g/L ethanol was obtained within 18 h and ethanol yield reached 94% of the theoretical yield.
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    Study on Comprehensive Extraction of Antioxidant and Essential Oil from Rosemary (Ⅰ)——Two-step Extraction
    BI Liang-wu;ZHAO Zhen-dong;LI Dong-mei;GU Yan;WANG Jing;LIU Xian-zhang
    2007, 27 (04):  11-15. 
    Abstract ( 585 )   PDF (909KB) ( 713 )   Save
    Two-step extraction with polar solvents and nonpolar solvents was an effective comprehensive extraction for antioxidant and essential oil of rosemary (Rosmarinus officinalis L. ). The method was simple on operation and was easily put into practice. The reasonable conditions of comprehensive extraction for antioxidant and essential oil of rosemary were as follows: broken rosemary leaves, 95% ethanol as polar solvent, 3-4 h of extraction at 90℃, and petroleum ether with the boiling range of 60-90℃ as nonpolar solvent. The yield of rosemary oil was 1.50%.Constituent analysis of rosemary oil showed that the essential oil belongs to that of Spanish type. The yield of rosemary antioxidant was 16.08%. The yield of rosemary antioxidant after decolorization by activated carbon was 85.00%. Main active components of rosemary antioxidant were carnosic acid, carnosol, and rosmarinic acid, whose average contents were 17.78%, 6.23% and 3.37%, respectively.
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    Study on Anti-tumor Activity of Extract from Masson's Pine Bark
    ZHENG Guang-yao;LI Ruo-da;WANG Cheng-zhang;XIE Heng;YE Jian-zhong;GAO Cai-xia
    2007, 27 (04):  16-20. 
    Abstract ( 698 )   PDF (873KB) ( 564 )   Save
    To study the anti-tumor activity of Masson's pine bark extract (MPBE) in vitro and in vivo, MTT assay was used to observe the growth inhibitory effect of MPBE on human colonic cancer cell line VoLo in vitro. The model of transplanted tumor in mice was used to observe the inhibiting effect on S180 sarcoma in mice, and the survival time of mice bearing Ehrlich ascites carcinoma (EAC), by calculating thymus and spleen indexes in mice bearing S180 sarcoma. Results showed: MPBE could inhibit the growth of LoVo cells in vitro, the inhibitory rates of MPBE at the concentration of 500 mg/L were 19.83%, 33.06% and 58.15% after incubation for 24, 48 and 72 h respectively; MPBE could significantly inhibit the growth of S180 sarcoma in mice, the inhibitory rates of MPBE were 30.2%, 37.8% and 42.3% at the dosags of 50, 100 and 200 mg/kg respectively. MPBE at the dose of 200 mg/kg could also increase the thymus and spleen indexes in mice bearing S180 sarcoma significantly. However, MPBE could not prolong the survival time of mice bearing Ehrlich ascites carcinoma. MPBE has obvious inhibitory effect on the growth of LoVo cells in vitro and S180 sarcoma in mice, it could be a potential chemopreventive or chemotherapeutic agent of cancer.
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    Study on Curing Reaction and Mechanical Properties of Epoxy Resin from Hydrogenated Terpinene-maleic Anhydride
    WU Guo-min;KONG Zhen-wu;CHU Fu-xiang;LU Ji-rong
    2007, 27 (04):  21-26. 
    Abstract ( 634 )   PDF (1176KB) ( 563 )   Save
    Hydrogenated terpinene-maleic ester type epoxy resin(HTME) is a type of epoxy resin synthesized from hydrogenated terpinene-maleic anhydride.The activity of curing reaction of HTME/methyl hexahydrophthalic anhydride (MeHHPA) system was investigated by means of DSC and gelation time determination.The curing behaviors of HTME/MeHHPA system were studied by qualitative analysis of FT-IR spectrum and quantitative analysis of curing degree determination.The mechanical properties of HTME cured with MeHHPA were compared with those of terpinene-maleic ester type epoxy resin (TME) andepoxy resin 6101 under the same condition. The results show that the reaction between HTME and MeHHPA was an exothermic one with reaction heat of 153.5 J/g and peak temperature at 157.9℃, and the HTME/MeHHPA system could be cured completely at 110℃ for 8 h with 0.5% benzyldimethylamine (BDMA) by weight of HTME as accelerant. The mechanic properties of the three kinds of cured epoxy products were about the same.
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    Studies on Lipophilic Chemical Constituents from Passiflora wilsonii Hemsl. Stem
    LI Gan-peng;YANG Li-juan;ZHAO Jing-feng;YANG Xiao-dong;LI Liang
    2007, 27 (04):  27-30. 
    Abstract ( 647 )   PDF (653KB) ( 535 )   Save
    From the stems of Passiflora wilsonii Hemsl., six compounds, namely 4-oxo-3,4-seco-A(1)-norfriedelan-2-oic acid (Ⅰ), 2-hydroxyl-3,4-seco-friedelan-3-oic acid ethyl-ester (Ⅱ), sitost-4-en-3-one (Ⅲ), 3-(2,4-dihydroxyphenyl)-2-propenoic acid (Ⅳ), glycerol 1-octadecanoate (Ⅴ), and 1-octacosanol (Ⅵ), were isolated from its lipophilic components and identified. Compound Ⅰ is a novel natural product, whose 13C NMR spectra were assigned for the first time. Compound Ⅱ is a new artificial compound.
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    Study on Liquefaction of Walnut Shell in Phenol and Application of Its Resinification Product as Wood Adhesives
    ZHENG Zhi-feng;ZOU Ju-chun;ZHANG Hong-jian;LING Min
    2007, 27 (04):  31-36. 
    Abstract ( 792 )   PDF (611KB) ( 695 )   Save
    Liquefaction of walnut shell in phenol using sulfuric acid as catalyst was investigated under different conditions of mass ratio of phenol to walnut shell, dosage of catalyst, reaction time and temperature. Results showed that with the increasing of phenol/walnut shell ratio from 2/1 to 5/1, the amount of residue decreased from 26.49% to 6.60%. With dosage of catalyst from 2% to 4%, reaction time from 5 to 120 min and temperature from 100 to 150℃, the amounts of residue decreased from 20.79% to 10.48%, 48.84% to 15.62% and 28.86% to 9.39%, respectively; the contents of unreacted free phenol decreased from 17.32% to 12.67%,41.71% to 10.25% and 21.94% to 14.33%, respectively too. Weight average molecular weight (MW) and degree of polydispersity of resultants of liquefaction decreased to 706-1 030, 1.04-1.25, respectively. The high-molecular weight part of liquefaction product decreased with increasing of phenol/walnut shell ratio, but increased with the increasing of H2SO4 concentration, reaction time and temperature. Compared to conventional phenol-formaldehyde (PF) resin adhesives, the liquefied walnut shell/phenol/formaldehyde co-condensed (WPF) resin can be used as adhesives for plywood with its bonding strength of 1.33 MPa.
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    Study on Complexation Properties of Black Wattle Tannin with Metals Ions
    SU Xiao-bao;DAI Li-jun;CHEN Shao-ping;LU Yu-dong;WU Zong-hua
    2007, 27 (04):  37-41. 
    Abstract ( 782 )   PDF (949KB) ( 768 )   Save
    Protonation constants and metal-complex stability constants of tannic acid, valonea tannin and black wattle tannin were determined by pH potentiometric titration under different temperatures in ionic strength I=0.1 mol/L NaCl solution. The complexation selectivities of different structures of tannins with Fe3+,Cu2+,Zn2+,Ni2+ ions were investigated and factors affecting protonation constant and stability constant were discussed. The results showed that the order of stability constants of the tannins complexed with Fe3+,Cu2+ ions was:black wattle tannin>valonea tannin>tannic acid, and that of tannins with Zn2+,Ni2+ ions was:valonea tannin>black wattle tannin> tannic acid. The rise of temperature was favorable for disassociation of phenol hydroxyl but unfavorable for the formation of complex. The purification of black wattle tannin by gel column chromatography showed little effect on the complex stability constants.
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    A New Method of Purifying Abietic Acid
    HAN Chun-rui;SONG Zhan-qian;SHANG Shi-bin
    2007, 27 (04):  42-46. 
    Abstract ( 720 )   PDF (948KB) ( 810 )   Save
    Abietic acid of 90.91% purity was obtained by amine salt method, using self-prepared amine A as raw material and 95% ethyl alcohol as recrystallization solvent. The method is economic and environmentally friendly because of the low price of amine A and small consumption of recrystallization solvent. Sample was characterized by 1H NMR, UV, IR and GC-MS methods.Purifications of abietic acid with isopropylamine, cyclohexylamine, octadecyl primaryamine, di-n-butylamine, triethylamine, and amine A were studied. The effects of carbon numbers of amines and primary, secondary, tertiary amines on purifying process were analyzed. The abietic acid with purity of 90% could be stored for 2 months at 5 kPa and -15℃.
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    Determination of Adsorption Film Thickness of Lignosulphonate and Modified Lignosulfonate on Coal Surface as Coal-water Slurry Additives
    ZHANG Yan-lin;QIU Xue-qing;YANG Dong-jie
    2007, 27 (04):  47-50. 
    Abstract ( 584 )   PDF (815KB) ( 594 )   Save
    It is introduced briefly the modification way and result of lignosulphonate (LS) as coal-water slurry (CWS) additive and determination of the adsorption film thicknesses of the LS and modified lignosulphonate (MLS) on the smooth surface of coal and microscopic slide by the method of elliptical polarization. The size of the space steric hindrance between LS and MLS adsorbing on the solid surface were quantitatively compared.Results showed that the adsorption film thickness of MLS is doubled comparied to LS. The thicknesses are different on the lyophobic surface and hydrophilic surface. It is favorable for the increase of the adsorption film thickness by increasing the lyophobic chain. The determination of adsorption film thickness verifies the validity of the modification result.
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    Studies on Polysaccharides and Flavonoids from Acanthopanax sessiliflorus( Rupr. et Maxim.) Seem. Fruit
    FENG Ying;MENG Xian-jun;WANG Jian-guo;WANG Jing-jing;ZHANG Qi
    2007, 27 (04):  51-54. 
    Abstract ( 635 )   PDF (758KB) ( 788 )   Save
    Acanthopanax sessiliflorus (Rupr. et Maxim.) Seem. has been used instead of A.senticosus in northeast region of China,but its active components are not very clear. In this article,the constituents of flavonoids and polysaccharides(ASP) from A.sessiliflorus fruit were studied by TLC and HPLC respectively. Using microemulsion as mobile phase on polyamide plate, nine constituents were separated from the flavonoids.Rf analysis showed one constituents to be hyperin, while rutin and quercetin were not found. The polysaccharides(ASP) were composed of Glc,Gal,Man,Fuc,Xyl,Rha,GlcN,GlcUA,GalUA and were mainly composed of four homogeneous polysaccharides whose molecular weights (Mr) are 21800,147000,45400,18100 respectively. Among them, the homogeneous polysaccharide ASP-Ⅰ was consisted of Gal and Rha in the molar ratio of 1:0.7,with Mr of 18100.The animal tests showed that ASP can increase the survival time under hypoxia condition and loaded swimming time of mice.
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    Preparation of Tung-nut-shell Based Activated Carbon and Its Adsorption Capacity for Organic Contaminants
    LIN Yun-zhu;QIAN Qing-rong;HUANG Bao-quan;GONG Bing-li;CHEN Qing-hua
    2007, 27 (04):  55-60. 
    Abstract ( 589 )   PDF (1116KB) ( 635 )   Save
    Activated carbon was prepared from tung-nut-shell by activation with zinc chloride at pyrolysis temperature of 400℃ for 1 h under nitrogen flow of 200 mL/min. The N2 adsorption-desorption isotherms of the prepared activated carbons were measured on a Beckman counter SA3100 surface area and pore size analysers, and the morphological structures of the activated carbons were observed by SEM. The prepared activated carbons were also employed as adsorbents for the experiment of adsorbing methylene blue and phenol in aqueous solutions. The results showed that the resultant activated carbons could be obtained from the tung-nut-shell with high BET surface area of 1 995 m2/g and high total pore volume of 1.521 mL/g, respectively. Increasing the mass ratio of ZnCl2 to tung-nut-shell resulted in the increment of the capacities for phenol and methylene blue adsorption. Compared to commercial activated carbon of F 400, the prepared activated carbon CT 3.0 exhibits higher capability for phenol and methylene blue adsorption. Therefore, it is expected to be a low-cost and efficient adsorption material for effluent treatment.
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    Study on Production of Fuel Ethanol from Poplar Hydrolyzate Obtained by Two-step Super-low Acid Hydrolysis
    ZHUANG Xin-shu;WANG Shu-rong;YUAN Zhen-hong;LUO Zhong-yang;WU Chuang-zhi;CEN Ke-fa
    2007, 27 (04):  61-65. 
    Abstract ( 645 )   PDF (963KB) ( 621 )   Save
    Choosing hydrolyzate of poplar as fermentation material, which was obtained by two-step super-low acids hydrolysis, fuel ethanol production was studied by using Candida tropicalis 2.637 and Saccharomyces cerevisiae 2.699 respectively. Simul-taneously the influences to the ethanol yield by various pretreatment methods, such as Ca(OH)2 neutralization, over-neutralization, active carbon adsorption and yeast-training were carried out. The experimental results show that C. tropicalis 2.637 is suitable to the first-step hydrolyzate rich in pentose to produce single cell protein. Yeast-training can improve fermentation speed and increase ethanol yield, especially to the second step hydrolyzate through which ethanol yield was increased from 14.45% to 39.37% by S. cerevisiae 2.699. The over-neutralization of hydrolyzate by Ca(OH)2 improved ethanol yield, too. Therefore,for the hydrolysis of the first-step hydrolyzate, which contains mainly pentose and accompanied with hexose, more ethanol can be obtained by C. tropicalis 2.637 than by S. cerevisiae 2.699.
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    Structural Characterization and Performance of Sulfodehydroabietic Acid Based Bis-quaternary Ammonium Cationic Surfactant
    CHEN Li-yun;FANG Gui-zhen;LIU Kai;HU Xu
    2007, 27 (04):  66-70. 
    Abstract ( 598 )   PDF (1039KB) ( 709 )   Save
    A new sulfodehydroabietic acid based bis-quaternary ammonium cationic surfactant (Ⅲ) was synthesized by sulfonation of dehydroabietic acid, followed by reaction with epoxypropyl triethyl ammonium chloride. Structures of products were characterized by IR.Surface activities of Ⅲ and the mixed system of sodium dodecyl sulphate (SDS) with Ⅲ were determined. Results show that content of sulfodehydroabietic acid is 92% by weight and content of cationic surface active substance is 91%. Critical micelle concentration (CMC) of Ⅲ is 1.1 mmol/L, and the foaming ability is 12 mm, showing a strong emulsification ability. Strong synergism of Ⅲ with SDS is observed, and the optimum synergism is obtained at the mass ratio of 1:3.
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    Continuous Fermentation of Pentose/Hexose Mixture by Immobilized Yeast to Prepare Ethanol
    JI Geng-sheng;YONG Qiang;YU Shi-yuan
    2007, 27 (04):  71-74. 
    Abstract ( 578 )   PDF (783KB) ( 595 )   Save
    Study on continuous fermentation of xylose/glucose mixture by Pichia stipitis under oxygen-limited condition to prepare ethanol was carried out. Mixture of 15.0 g/L xylose and 30.0 g/L glucose as substitute of lignocellulosic hydrolyzate, was used as main fermentation substrate. Tow-stage fermentation cultures were carried out in a two-reactor system under condition of temperature of 35℃ and a ventilation rate of 100-150 mL/min. The working volume of single reactor was 1.5 L. When the influent rate was ca. 60 mL/h, average ethanol concentration in the effluent was 13.79 g/L, and the utilization rate of reducing sugar was 83.09%. When the influent rate was changed to ca. 45 mL/h average ethanol concentration in the effluent was 15.41 g/L, and the utilization rate of reducing-sugar was 90.38%. Using immobilization and low pH value treatment method, the system was run steadily and no contamination was found during a 35-day research.
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    Primary Research on the Core-shell Structure of Turpentine-polystyrene Particles
    LIN Ming-tao;CHU Fu-xiang;LU Ji-rong;LIU Mei-hong;WANG Ji-fu;MA Li;WANG Chun-peng
    2007, 27 (04):  75-78. 
    Abstract ( 564 )   PDF (899KB) ( 508 )   Save
    Turpentine is a natural product of pine and a kind of important fine chemical material. Polymeric microsphere can act as micro-reactor or the carrier of medicament or essence, etc, receiving great research interest recently. In this paper, the steady monodispersed nanometric styrene monomer droplets containing turpentine were prepared by ultrasonic dispersion method. Then polymerization was carried out in the presence of oil-dissolved initiator and the turpentine-polystyrene hybrid particles were prepared. Phase separation between polystyrene and turpentine was occurred, the polymeric particles with the structure of polystyrene as shell and turpentine as core were produced during polymerization. The core-shell structure was confirmed by transmission electronic microscopy and GC-MS analysis.
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    Study on Synthesis and Properties of Biodiesel Oil from Rosin
    NIE Xiao-an;JIANG Jian-chun;DAI Wei-di;CHANG Xia
    2007, 27 (04):  79-81. 
    Abstract ( 575 )   PDF (553KB) ( 724 )   Save
    Synthesis technology of biodiesel oil from rosin was studied, and its combustion properties were analyzed. The result showed that liquid abietane could be synthesized from rosin under the condition of reaction temperature 270℃,reaction time 2 h and catalyst dosage 10%. Through scientific prescription, the biodiesel oil from abietane exhibited an hexadecane number of 52 and sulfur content of 0.004% which meet the required standard.The study has profound practical significance of application.
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    Enzymatic Hydrolysis Characteristics of Xylanases in Ultrafiltration Membrane Reactor
    JIANG Hua;XU Yong;YU Shi-yuan
    2007, 27 (04):  82-86. 
    Abstract ( 590 )   PDF (862KB) ( 550 )   Save
    It was comparatively investigated that xylan was hydrolyzed by crude and purified xylanases in ultrafiltration membrane reactor (UMR) and conventional stirring batch reactor (CSBR). After enzymatic hydrolysis of 525 min in UMR using crude or purified xylanases,the obtained individual oligosaccharide components (xylobiose, xylotriose, xylotetraose, and xylopentaose) in the hydrolysates accounted for some 20% respectively, and xylose about 9.5%. The xylo-oligosaccharide yields, the ratio of xylo-oligosaccharides to total saccharides, and the productivity of xylo-oligosaccharides in UMR using crude xylanases were 18.7%,14.9% and 16.0% higher than those in CSBR using purified xylanases, respectively, but xylose yield was 55.5% lower than that in the latter case. The amount of individual oligosaccharide component in UMR was almost equal in the UF membrane reactor using crude xylanases, and more xylobiose was obtained in the CSBR using purified xylanases. Therefore,high-quality xylo-oligosaccharides could be prepared using crude xylanase in UMR.
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    Characteristics of Adsorption of Pb2+ from Effluents onto Activated Carbon Prepared from Coconut Shell by Microwave Heating
    ZHANG Yong;NING Ping;GAO Jian-pei;PENG Jin-hui;ZHANG Li-bo;YANG Kun-bin;XIA Hong-ying
    2007, 27 (04):  87-91. 
    Abstract ( 551 )   PDF (958KB) ( 655 )   Save
    Adsorption of Pb2+ from aqueous solution onto activated carbon prepared from coconut shell by microwave heating(MAC) was investigated in a batch system. The effects of temperature on adsorption thermodynamics were studied. Thermodynamic parameters such as standard Gibbs free energy (ΔGΘ), standard enthalpy (ΔHΘ), and standard entropy (ΔSΘ) were evaluated by applying the Van't Hoff equation. The thermodynamics of Pb2+ adsorption onto activated carbon indicates that it is of spontaneous and exothermic nature. Langmuir and Freundlich isotherms were used to analyze the equilibrium data at different temperatures and the equilibrium data were found to be well represented by the Langmuir isotherm equation.
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    Synthesis of Nateglinide as an Antidiabetic Drug from β-Pinene
    MA Shi-ying;SHEN Min-min;HA Cheng-yong;GAO Hong-yun;
    2007, 27 (04):  92-96. 
    Abstract ( 827 )   PDF (865KB) ( 743 )   Save
    Starting from β-pinene, nateglinide was synthesized through oxidation, acid-catalytic rearran-gement, hydrogenization, isomerization and acylation. The chemical structure of the target compound is confirmed by IR, 1H NMR, 13C NMR, MS. Nateglinide was successfully synthesized by using natural product as starting material,via six steps in a total yield of 28.1% with the advantages of simple operation and low cost.
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    Study on the Degradation of Wheat Bran by Bacillus licheniformis
    YAN Hong;YANG Qian
    2007, 27 (04):  97-102. 
    Abstract ( 548 )   PDF (1373KB) ( 779 )   Save
    The degradation of wheat bran by Bacillus licheniformis(Bacillus sp. X18) was studied by means of measuring concentrations of reducing sugar and soluble total sugar, activities of cellulase and hemicellulase in fermented broth, weight loss, crystallinity, FT-IR spectra and surface structure of residue. The results showed that the process of biodegradation of lignocellulose is actually simultaneous saccharification and fermentation. Cellulase and hemicellulase activities reached the highest level in 96 and 48 h, respectively. Concentrations of soluble total sugar and reducing sugar reached the highest level in 4 and 48 h,at 5257.79 and 1363.94 mg/L, respectively, and then decreased with time and maintained invariable value. Crystallinity of residue had no obvious change after 5 d cultivation. FT-IR spectrum of residue showed that Bacillus sp. X18 mainly degradated cellulose in wheat bran. After 5 d cultivation degradation rates of cellulose, hemicellulose and lignin in wheat bran were 37.03%, 15.86% and 17.03%, respectively. SEM of surface structure of degradated wheat bran by Bacillus sp. X18 showed that constituent serving function of support in framework of honeycombed structure was mainly degradated.
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    Research on Difference of Betulin Content in Different Parts and Provenances of Birch (Betula platyphylla Suk.)
    FAN Gui-zhi;ZHAN Ya-guang;WANG Bo;QIU Lei;LIU Gui-feng;WANG Hui-ren
    2007, 27 (04):  103-106. 
    Abstract ( 570 )   PDF (794KB) ( 702 )   Save
    To understand the difference of the betulin content in different parts and provenances in Betula platyphylla Suk., the methods to extract betulin were selected, and an accurate HPLC method to detect betulin content was used. The results were as follows:Betulin contents of the same birch bark through 4 extraction methods,namely Soxhlet extraction, supersonic wave, extraction refluxing and chloroform extraction were 240.25, 239.57, 207.88 and 194.09 mg/g respectively; The contents of betulin in different parts of birch were outer bark>branch bark>inner bark>bud>leaf>root>pollen; Betulin contents in the bark of eight-year old birches of 13 provenances were detected, and their range was from 132.45 to 257.11 mg/g. Analyzing the relations among betulin content and growth status, geographical location and climatic factors, it was found that the effect of growth status on betulin content was not significant, and betulin content was not only affected by self-provenance and heredity background but also by geographical location and climatic factor.
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    A Novel Strategy for Synthesizing Campholenonitrile and Campholenate Perfumes
    PAN Cheng-xue;WANG Bi-hua
    2007, 27 (04):  107-110. 
    Abstract ( 621 )   PDF (821KB) ( 587 )   Save
    Synthetic camphor was reacted with hydroxylamine to give camphor oxime (81% yield). The resulted oxime was refluxed in 25% sulfuric acid to undergo Beckmann fragmentation to form campholenonitrile in 82% yield. Alcoholysis of campholenonitrile in different alcohols catalyzed by dry hydrogen chloride resulted in five campholenate perfumes of excellent yields (82%-91%). All target compounds were characterized by means of 1H NMR, IR and elemental analysis. Among these compounds campholenonitrile possessed strong woody and ethyl campholenate fruity smell, which has promised application prospects. The novel synthetic process has the significant advantages of cheap and commonly available raw materials, mild reaction condition, simple operation and high yield.
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    Study on Super-high-pressure Extraction of 2α-Hydroursolic Acid from Lagerstroemia speciosa (L.) Pers. Leaves
    ZONG Wei;ZHAO Guang-yuan;ZHANG Wen-ye
    2007, 27 (04):  111-114. 
    Abstract ( 628 )   PDF (821KB) ( 732 )   Save
    The super-high-pressure (SHP) extraction of 2α-hydroursolic acid from leaves of Lagerstroemia speciosa (Linn.) Pers. was studied. The optimum extraction condition was optimized with orthogonal test by using L9(34) orthogonal design with extractive yield of 2α-hydroursolic acid as index, investigating the influences of SHP pressure, time, ethanol concentration and the ratio of solid to liquid. Optimum extraction conditions were determined as follows: SHP pressure 300 MPa, SHP time 5 min, 90% ethanol as extracting solvent, stock ratio 1:15 (g:mL), extracting for three times.The yield of 2α-hydroursolic acid was 0.415%.
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    Experimental Study on Preservation Performance and Acute Toxicity of Maackia amurensis Rupr.et.Maxim. Heartwood Extracts
    SU Wen-qiang;YANG Dong-mei;LI Jian
    2007, 27 (04):  115-119. 
    Abstract ( 512 )   PDF (966KB) ( 604 )   Save
    The heartwood and bark of Maackia amurensis Rupr.et.Maxim. were used as raw material to obtain 10 kinds of extracts by extracting with ether, chloroform, acetone, methanol and water,respectively. Antibacterial activities against Coriolus versicolor and Gloeophyllum trabeum of 10 kinds of extracts were studied, It was found that methanol and acetone extracts of heartwood have good antibacterial activities. Wood preservation activities of methanol extract of heartwood was also compared with the wood preservative acid copper chromate(ACC) in lab. Weight loss and scanning electron microscopy (SEM) photography showed that methanol extract of heartwood has better decay resistance against C. versicolo, weaker decay resistance against G. trabeum,but ACC has better decay resistance against two epiphytes. The acute toxicities of methanol extract of heartwood and ACC to Brachydanio rerio were studied. At 24,48 and 72 h, LC50 of methanol extract were 16.5, 12.7, 12.0 mg/L respectively, LC50 of ACC were 3.2, 2.5, 2.0 mg/L respectively. The safety concentrations of methanol extract and ACC are 2.26 and 0.46 mg/L respectively.
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    Separation and Purification of Flavonoid from Lithocarpus polystachyus (Wall.) Rehd. with Macro-porous Resin ADS-7
    DONG Hua-qiang;NING Zheng-xiang;LI Lin;YU Li-jing;LIN Li-chao
    2007, 27 (04):  120-122. 
    Abstract ( 525 )   PDF (659KB) ( 655 )   Save
    The flavonoid was separated and purified from the crude extract of Lithocarpus polystachyus(Wall.) Rehd. leaves with macro-porous resin (MPR) ADS-7, and the technology conditions were investigated in this experiment. The results showed that the optimum condition of the technology was that the ratio of the crude extract solution/resin was a little bigger than 3, static adsorption time was 2 h at neutral pH value, 1 500 mL 80% (volume fraction) ethanol as eluant, and eluation speed was 500 mL/h. By this technology the flavonoid content was increased from 40% of the crude extract to 88% of the purified product and the yield was 91%.
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    Study on Synthesizing Terpinyl Acetate by Microwave Irradiation
    WU Chun-hua;ZHANG Jia-yan;ZHAO Qian-rong;AN Xin-nan
    2007, 27 (04):  123-126. 
    Abstract ( 642 )   PDF (716KB) ( 553 )   Save
    The technology of synthesizing terpineyl acetate has been studied by using the method of batch-wise microwave irradiation. The results showed that the optimized conditions were as the follows: ratio of acetic anhydride to terpineol was 1.25:1, 4% acetic anhydride and phosphoric acid were used as catalyst (based on terpineol mass) under 100 W microwave, and irradiation time was 2 h. The conversion of terpineol was 96.92% and the yield of terpineyl acetate was 86.53% under optimum conditions. Compared with normal methods, it had higher efficiency, only one eighth reaction time of normal method was needed.
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    Study on Preparation of Activated Carbon from Tobacco Stems
    LU Chun-lan;XU Shao-ping;LIU Shu-qin;QI Ben-dong;LIU Chang-hou;CHI Ji-an
    2007, 27 (04):  127-130. 
    Abstract ( 600 )   PDF (642KB) ( 755 )   Save
    Activated carbon was prepared from tobacco stem by steam activation. The results show that activation temperature and S/C ratio are important to the porosity development of the activated carbon. Activated carbon with BET surface area of 522-590 m2/g and iodine adsorption capacity of 840-912 mg/g has been produced under activation temperature 750-800℃ and S/C ratio between 1.5-2.0:1.0. The study confirms that tobacco stems are highly reactive to steam activation, and therefore can be used to produce activated carbon through a single stage activation process in a fluid bed. Mineral matters in tobacco stems were found to be catalytic to steam activation of the precursor, upon which a process of deashing with diluted HCl solution followed by activation to produce activated carbon with relatively lower mineral content has been put forward.
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