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多酚羧酸合成功能高分子材料研究
添加时间: 2010-1-23 10:29:34 文章来源: 文章作者: 点击数:4737
 

(Ⅱ)

——没食子酰化改性纤维素合成及其功能特性试验

汪咏梅,陈笳鸿*,吴冬梅,吴在嵩,王成章

(中国林业科学研究院林产化学工业研究所;国家林业局林产化学工程

重点开放性实验室,江苏南京210042



摘 要:以没食子酰基为功能基团,以改性纤维素为骨架合成功能高分子材料没食子酰化改性纤维素(没食子酰基-1,6-己二亚胺基-羟丙基-纤维素,CG):先将纤维素与环氧氯丙烷反应,然后依次接上己二胺桥链和三乙酰基没食子酰基,最后将没食子酰基脱去乙酰基得到目标产物。功能试验表明,1 g产物能结合明胶49.5 mg,并可再生使用。1 g产物络合金属离子的能力:Fe3+ 53.4 mgCu2+ 38.7 mgHg2+ 46.5 mgMn2+ 6.8 mgZn2+ 27.9 mgPb2+ 57.2 mg。产物在稀酸、稀碱、稀醇和热水中具有稳定性。

关键词:功能高分子材料;没食子酰化改性纤维素;纤维素;多酚羧酸;没食子酰基

中图分类号:TQ943TQ352   文献标识码:A   文章编号:0253-2417(2007)02-0001-06

 

Synthesis of Functional Polymer Material with Polyphenolic Acid ()

——Synthesis and Functional Test of Galloyl Modifiedcellulose

WANG Yong­meiCHEN Jia­hongWU Dong­meiWU Zai­songWANG Cheng­zhang

(Institute of Chemical Industry of Forest ProductsCAFKey and Open Lab.on Forest Chemical EngineeringSFA,  Nanjing 210042China)

 

Abstract: A new type of functional polymer material, galloyl modified­cellulosegalloyl­1,6­hexyldiimino­oxypropyl­cellulose, CG ), was synthesized with phenolic acid as functional group and modified cellulose as molecular skeleton. The synthesis procedure was as follows: cellulose was first reacted with epichlorohydrin, then the hexyl diamine bridge chain and triacetyl­galloyl group were successively connected, and finally the galloyl group was deacetylated. Functional tests indicated that 1 g of CG could adsorb 49.5 mg of gelatin and be reusable after regeneration, and complex the metallic ions such as: Fe3+ 53.4 mg, Cu2+ 38.7 mg, Hg2+ 46.5 mg, Mn2+ 6.8 mg, Zn2+ 27.9 mg, Pb2+ 57.2 mg, respectively. The product CG was stable in dilute acidic, alkaline, ethanolic solutions and hot water.

Key words:functional polymer material;galloyl modified­cellulose;cellulose;

polyphenolic acid;galloyl group

 

 

 

松香歧化纳米镍负载型催化剂的失活原因及再生工艺研究

王亚明,王 震,蒋丽红,王路辉,罗康碧,束嘉秀

(昆明理工大学生物与化学工程学院,云南昆明650224)

摘 要:用醇盐水解法制得纳米镍负载型松香歧化新型催化剂,用此催化剂催化松香歧化,考察了催化剂的寿命。用扫描电镜、原子吸收分光光度法、X射线衍射光谱、比表面积测定等手段研究了该催化剂失活的原因,筛选出该催化剂再生的最佳工艺条件:焙烧过程通入空气和氮气,焙烧温度450 ℃,时间2 h,催化剂还原温度300 ℃。用此方法反复再生5次,催化剂性能基本保持不变。

关键词:纳米粒子;镍负载催化剂;松香歧化反应;失活;再生

中图分类号:TQ351.471TQ426   文献标识码:A   文章编号:0253-2417(2007)02-0007-04

 

Study on Deactivation and Regeneration of Ni­loaded Nanocatalyst for Disproportionation of Gum Rosin

WANG Ya­ming, WANG Zhen, JIANG Li­hong, WANG Lu­hui, LUO Kang­bi, SHU Jia­xiu

(Institute of Biological and Chemical Engineering,Kunming University of Science and Technology, Kunming 650224, China)

 

Abstract: Ni­loaded nanocatalyst has been prepared by means of metal alkoxide hydrolysis. The lifetime of the catalyst for catalyzing disproportionation of gum rosin is investigated. The cause of deactivation was investigated by TEM, AAS, XRD and BET. The conditions for regeneration of the catalyst, such as calcination temperature, calcination time, calcination environment, reduction temperature are respectively studied. The activity of catalyst  could be kept constant for 5 times of regeneration under the conditions of air+N2 stream during calcination at  temperature 450 , calcination time2 h, reduction temperature 300 .

Key words:nanometer particle;Ni­loaded catalyst;disproportionation of gum rosin;deactivation;regeneration

 

 

 

乙酸龙脑酯标准样品的制备和定值研究

赵振东1,李冬梅1,毕良武1,王 婧1,曹向民2,古 研1

1. 中国林业科学研究院林产化学工业研究所;国家林业局林产化学工程重点开放性实验室,江苏南京210042 2. 九江市出入境检验检疫综合技术中心,江西九江332000

 

摘 要:研究了乙酸龙脑酯标准样品的制备、均匀性和稳定性及其定值方法。乙酸龙脑酯标准样品的制备采用高纯度天然龙脑的乙酰化法,乙酸龙脑酯标准样品的含量测定采用气相色谱面积归一化法,制备得到的乙酸龙脑酯标准样品通过了均匀性检验,且至少在24个月内是稳定的。乙酸龙脑酯标准样品的多实验室联合定值结果表示为:乙酸龙脑酯含量的标准值99.93 %;标准不确定度0.08 %;扩展不确定度(95 %置信率) 0.16 %

关键词:乙酸龙脑酯;标准样品;定值

中图分类号:TQ351.4   文献标识码:A   文章编号:0253-2417(2007)02-0011-05

 

Study on Preparation and Certification of Reference Substance of Bornyl Acetate

ZHAO Zhen­dong1LI Dong­mei1BI Liang­wu1 WANG Jing1CAO Xiang­min2GU Yan1

1. Institute of Chemical Industry of Forest Products,CAF;Key and Open Lab. on Forest Chemical Engineering,SFA,Nanjing 210042, China; 2. General Technical Center of Jiujiang Entryexit Inspection and Quarantine, Jiujiang 332000, China

 

Abstract: Preparation, homogeneity, stability and certification of reference substance of bornyl acetate were studied. The reference substance of bornyl acetate was prepared by  acetylation of highly pure borneol isolated and purified from a natural borneol product. The content of bornyl acetate in reference material was measured by gas chromatographic area normalization. The reference substance of bornyl acetate passed the test of homogeneity, and it was stable during 24 months at least. The joint certification results of bornyl acetate reference substance through multiple labs showed that the standard value of bornyl acetate content was 99.93 %with  standard uncertainty of 0.08 %, extended uncertainty of  0.16 %and confidence coefficient of 95 %.

Key words:bornyl acetate;reference substance;certification

 

 

 

壳聚糖微球固定化β-葡萄糖苷酶的研究

朱均均, 江小华,   , 余世袁

(南京林业大学化学工程学院,江苏南京210037



摘 要:以壳聚糖微球为载体,采用吸附-交联法固定化β-葡萄糖苷酶。采用正交试验设计确定最佳固定化条件。β-葡萄糖苷酶的最佳固定化条件为:pH5.0,酶用量48.6 IU/g(以绝干壳聚糖计,下同)的β-葡萄糖苷酶经壳聚糖微球吸附12 h后,在 25 ℃、 1.0 %的戊二醛存在下交联2 h,得到酶活力为41.76 IU/g和酶活回收率为85.93 %的固定化酶。

关键词:壳聚糖;β-葡萄糖苷酶;固定化

中图分类号:TQ920.1;Q814.2   文献标识码:A   文章编号:0253-2417(2007)02-0016-05

 

Immobilization of β­glucosidase on Chitosan Beads

ZHU Jun­jun, JIANG Xiao­hua, YONG Qiang, YU Shi­yuan

(College of Chemical Engineering,Nanjing Forestry University, Nanjing 210037, China)

 

Abstract: β­Glucosidase was immobilized on chitosan beads by adsorption and crosslinking. The method of orthogonal test was used to investigate the optimal condition of immobilization. The optimal condition of immobilization was as follows: β­glucosidase dosage 48.6 IU/g dry chitosan was absorbed with chitosan beads at pH value 5.0 for 12 h, followed by crosslinking at 25 for 2 h in 1.0 %glutaraldehyde(GA) solution. The activity of immobilized β­glucosidase and recovery rate of β­glucosidase activity were 41.76 IU/g (based on dry chitosan) and 85.93 %, respectively.

Key words:chitosan;β­glucosidase;immobilization 

 

 

 

Preparation of Cationic Dispersed Rosin Sizing Agent

LI Shu­jun1SONG Zhan­qian2

(1. Key Laboratory of Biobased Material Science and Technology,Northeast Forestry University,Ministry of Education, Harbin 150040, China; 2. Institute of Chemical Industry of Forest Products, CAF;Key and Open Lab. on Forest Chemical Engineering, SFA, Nanjing 210042, China)



Abstract: Cationic dispersed rosin sizing agent (CDRS) was prepared by changing ionic characteristics and its properties were characterized. The cationic agent used was modified from a non­ionic polymer. The product CDRS was a uniform emulsion of white color, +26 mV Zeta­potential, 0.271 μm volume average particle diameter, 0.404 uniformity and good particle diameter distribution. Under the condition of pH value 6.0 and Al2(SO4)3 dosage 1.0 %, CDRS showed comparable sizing degree of 40 s for regenerated pulp and better anti­aging permanence in comparison with the control (Hi­phase 35). The results of turbidity and SEM observation showed that the sizing efficiency of CDRS decreased quickly with the raising of pH value because of the free rosin saponification. The results indicate that CDRS has a promising future with its low cost, easy preparation and significant sizing effect under nearly neutral conditions.

Key words: cationic dispersed rosin sizing agent;modified cationic agent;sizing efficiency

CLC numbers:TQ351.471;TS727 Document code:A Article ID: 0253-2417(2007)02-0021-04

 

阳离子型松香施胶剂的制备

李淑1,宋湛谦2

1.东北林业大学生物质材料科学与技术教育部重点实验室,黑龙江哈尔滨150040;2.中国林业科学研究院林产化学工业研究所;国家林业局林产化学工程重点开放性实验室,江苏南京210042

 

摘 要:以非离子型聚合物改性得到阳离子化剂,通过转型法成功制得了阳离子型分散松香施胶剂(CDRS),并对其性质进行了表征。CDRS为白色均一乳液,其Zeta电位为+26 mV,体积平均粒径为0.271μm,一致性为0.404,粒径分布较好。在pH6.0Al2(SO4)3用量1 %的条件下,CDRS对再生纸浆的施胶度为40s,施胶效果接近对照样品,耐老化性能则优于对照样品Hi-phase 35。浊度实验和扫描电子显微镜观察表明,由于游离松香的皂化作用,CDRS的施胶效果随着pH值的升高而迅速下降。由于成本低,制备方法简单,在近中性条件下施胶效果较好。

关键词:阳离子型松香施胶剂;改性阳离子化剂;施胶效果

 

 

 

脱氢松香酸甲酯喹啉衍生物的合成与表征

张 业,潘英明,王恒山*,陈 清,廖永志,潘伟龙

(广西师范大学化学化工学院,广西桂林541004

 

摘 要:以脱氢松香酸甲酯(Ⅱ)为起始原料,通过在12位溴代得到12--脱氢松香酸甲酯(Ⅲ),再经过在13位选择性硝化后还原制得中间体13-氨基脱异丙基脱氢松香酸甲酯(),Ⅴ继续与甘油在浓硫酸作用下缩合得(4R, 12bS-4, 12b-二甲基-1, 2, 3, 4, 4a , 5, 6, 12b-八氢化萘并[1, 2-g]喹啉-4-羧酸甲酯()和(7R,10aS-7, 10a-二甲基-5, 6, 6a, 7, 8, 9, 10, 10a-八氢化萘并[2, 1-f]喹啉-7-羧酸甲酯()两种松香基喹啉衍生物,这两种产物的产率分别为51.2 % 20.3 %,质量分数分别为71.6 % 28.4 %,产物的结构通过IR1H NMR和元素分析进行了表征。

关键词:脱氢松香酸甲酯;喹啉

中图分类号:TQ351   文献标识码:A   文章编号:0253-2417(2007)02-0025-04

 

Synthesis and Characterization of Two Quinoline Derivatives from Dehydroabietic Acid

ZHANG Ye, PAN Ying­ming, WANG Heng­shan, CHEN Qing, LIAO Yong­zhi, PAN Wei­long

(School of Chemistry and Chemical Engineering,Guangxi Normal University, Guilin 541004, China)

 

Abstract: Two quinoline derivatives from dehydroabietic acid were synthesized. Methyl dehydroabietate () was bromated at 12­position to give methyl 12­bromo­dehydroabiete (Ⅲ). From ,methyl 13­aminodeisopropyldehydroabietate () was synthesized by nitration with nitric acid and hydrogenation in the presence of H2 and Pd/C. Then was further converted into two quinoline derivatives, namely methyl (4R,12bS)­4, 12b­dimethyl­1, 2, 3, 4, 4a, 5, 6, 12b­octahydronaphtho 1, 2­g quinoline­4­carboxylate () and methyl (7R,10aS)­7, 10a­dimethyl­5, 6, 6a, 7, 8, 9, 10, 10a­octahydronaphtho 2, 1­f quinoline­7­carboxylate (), by condensation with glycerol in the presence of concentrated sulfuric acid. The yields were 51.2% and 20.3 %, and the mass fraction were 71.6 %and 28.4 %,respectively. Their structurs were characterized by IR, 1H NMR and elemental analysis. 

Key words: methyl dehydroabietate;quinolines

 

 

 

木材苯酚液化产物制备碳纤维的初步探讨

马晓军1,2,赵广杰2

1.天津科技大学包装与印刷工程学院,天津300222;

2.北京林业大学材料科学与技术学院,北京100083

 

摘 要:为拓宽木材液化产物的应用领域,提高木材产品的附加值,实现木材的高效利用,在研究木材苯酚液化产物特性的基础上,提出了木材苯酚液化产物碳纤维材料的制备构思和工艺路线。利用木材苯酚液化产物为前驱体,通过加入反应剂如六次甲基四胺等调制纺丝液,熔融纺丝后将纤丝在甲醛和盐酸混合溶液中加热固化形成网状交联结构,然后在惰性气体保护下高温炭化制备成碳纤维,同时对制备过程中可能存在的影响因素进行了分析。

关键词:木材苯酚液化;木材纤维;碳纤维

中图分类号:TQ35   文献标识码:A   文章编号:0253-2417(2007)02-0029-04

 

Preliminary Study on Preparation of Carbon Fiber from Woodphenol Liquefaction Products

MA Xiao­jun1,2, ZHAO Guang­jie2

(1. College of Packaging & Printing Engineering,Tianjin University of Science & Technology, Tianjin  300222, China;2. College of Material Science and Technology,Beijing Forestry University, Beijing 100083, China)

 

Abstract: In order to widen the application of wood liquefaction products, to improve the added value of wood products, and to realize the highly effective uses of wood, on the basis of studying the characteristics of phenolated wood, the ideas of preparing  carbon fiber from wood­phenol liquefaction products and its technical route were proposed. Wood liquefaction products in phenol was used as precursor to prepare spinning solution by mixing with reactant such as HMTA.The filaments prepared by meltspinning was heated and solidified by soaking in an acid solution containing HCl and HCHO as main components to form the network crosslinking structure. Finally the filaments were carbonized into carbon fibers at high temperature under a stream of inert gas.Besides, some influencing factors in the course of preparation were analyzed. 

Key words:wood­phenol liquefaction;wood fiber;carbon fiber

 

 

 

 

桐油酸酐酰亚胺酚醛树脂耐热性研究

商士斌,王 瑀,宋湛谦,王 丹

 (中国林业科学研究院林产化学工业研究所;国家林业局林产化学工程重点开放性实验室,江苏南京210042)



摘 要:以桐油、马来酸酐、双马来酰亚胺及酚醛树脂为基本原料,合成了具有较好耐热性的桐油酸酐酰亚胺酚醛树脂。重点讨论了不同原料,如桐油、马来酸酐、双马来酰亚胺及酚醛树脂的用量、固化反应温度及固化反应时间等因素对树脂耐热性的影响。当桐油、双马来酰亚胺、马来酸酐和酚醛树脂的质量比为10.20.150.25, 170 ℃烘烤4 h固化时,所得树脂具有较好的耐热性,温度指数(T20000)可达165.8 ℃。

关键词:桐油;双马来酰亚胺;酚醛树脂;马来酸酐;耐热性能

中图分类号:TQ323   文献标识码:A   文章编号:0253-2417(2007)02-0033-03

 

Thermal Stability of Bismaleimide­phenol Formaldehyde Resin Modified by Tung Oil­maleic Anhydride Adduct

SHANG Shi­bin, WANG YuSONG Zhan­qian, WANG Dan

(Institute of Chemical Industry of Forest Products,CAFKey and Open Lab.on

Forest Chemical EngineeringSFA,  Nanjing 210042, China)

 

Abstract: A modified phenol formaldehyde resin with high thermal stability was prepared from tung oil, maleic anhydride (MA) bismaleimide (ABMI),and phenol formaldehyde resin (PF). Effects of amounts of each component and the curing condition were investigated.The optimum conditions are: mass ratio of tung oil/bismaleimide/

maleic anhydride/PF 10.200.150.25, curing temperature 170 and curing time 4 h. The temperature indexT20000 can reach 165.8 .

Key words:tung oilbismaleimidephenol formaldehyde resinmaleic anhydride;thermal stability

 

 

 

磷酸法竹质颗粒活性炭的制备研究

王志高,蒋剑春,邓先伦,常 侠,童娅娟,刘汉超

(中国林业科学研究院林产化学工业研究所; 国家林业局林产化学工程重点开放性实验室,江苏南京210042

 

摘 要:以竹屑为原料,采用磷酸法活化,制得了中微孔发达的颗粒活性炭:A法焦糖脱色率70 %,亚甲基蓝吸附值 210 mg/g,碘吸附值1 100 mg/g以上,丁烷工作容量132g/L,强度95 %以上。其孔分布以中微孔为主(Rn2.6 nm), 达到了86.3 %。适合于液体脱色精制和汽油蒸气的回收之用。对制备过程中捏合温度和时间、捏合过程中有无空气参与反应以及活化温度等工艺对颗粒活性炭性能的影响进行了研究考察,发现捏合过程中空气参与反应有利于造就发达的中微孔结构,活化温度的提高(500 )使得孔分布向着微孔方向发展。并通过改进捏合工艺和添加催化剂,使得颗粒活性炭的性能和表观光洁度得到提高。

关键词:竹屑;颗粒活性炭;脱色;汽油蒸气

中图分类号:TQ424.19   文献标识码:A   文章编号:0253-2417(2007)02-0036-05

 

Study on Preparation of Granular Activated Carbon from Bamboo Sawdust  Activated with H3PO4

WANG Zhi­gao, JIANG Jian­chun, DENG Xian­lun, CHANG Xia, TONG Ya­juanLIU Han­chao

(Institute of Chemical Industry of Forest Products,CAF;Key and Open Lab. on Forest Chemical Engineering,SAF,  Nanjing 210042, China)

 

Abstract: Granular activated carbon (GAC) was made from bamboo sawdust by activation with H3PO4.The properties of the product are: decolorization of caramel A 70 %; methylene blue  adsorption 210 mg/g; iodine number 1 100 mg/g,n­butane working capacity (BWC) 132g/L; abrasive resistance 95 %. It exhibits a high percentage of microporosity and mesoporosity(Rn2.6 nm,amounting to 86.3 %, which can be applied to decolorize and refine  liquid, and recover gasoline vapor. Effects of affecting factors in preparing process, such as temperature and time of kneading, with or without air participation during kneading, and activation temperature on the properties were investigated. It was found that air participation in reaction during kneading contributes greatly to create a high percentage of microporosity and mesoporosity, and increased activation temperature (500 ) can lead to develop micropores. Moreover, with improvement on kneading and adoption of catalysts, both properties and surface smoothness of GAC were  improved greatly.

Key words:bamboo sawdust;granular activated carbon;decolorization of liquid;gaso­

line vapor

 

 

 

槐花米抗氧化成分的提取及其活性研究

潘英明1,梁 英2,朱志仁1,王恒山1,韦小芳1,梁 敏1

1.广西师范大学化学化工学院,广西桂林5410042.桂林电子工业学院八系,广西桂林541004



摘 要:75 %乙醇提取了槐花米中具有抗氧化活性的粗提物,然后通过碱提酸沉法从该粗提物中提取了芦丁,并制备了芦丁的水解产物槲皮素。采用磷钼酸盐法测定了不同质量浓度的粗提物、芦丁和槲皮素的抗氧化活性,并与BHTVC的抗氧化活性进行了比较。结果表明,抗氧化性强弱顺序为:VC>槲皮素>芦丁>粗提物>BHT

关键词:槐花米;芦丁;槲皮素;抗氧化活性

中图分类号:TQ91   文献标识码:A   文章编号:0253-2417(2007)02-0041-04

 

Study on Extraction and Activity of Antioxidant Components from Sophra japonica L.

PAN Ying­ming1, LIANG Ying2, ZHU Zhi­ren1, WANG Heng­shan1, WEI Xiao­fang1, LIANG Min1

(1. School of Chemistry and Chemical Engineering,Guangxi Normal University, Guilin 541004, China;2.The Eighth Department,Guilin Institute of Electronic Technology, Guilin 541004, China)

 

Abstract: Crude extracts were extracted from Sophra japonica L.with 75 % alcohol.Rutin was obtained from the crude extracts by alkine extraction and acid precipitation.Quercetin was prepared by hydrolyzing rutin.Their antioxidant activities were tested using phosphomolybdate method, and compared with those of BHT and VC.The results showed their antioxidant activities are in the sequence of VCquercetinrutincrude extractsBHT.

Key words:Sophra japonica L.;rutin;quercetin;antioxidant activity

 

 

 

青橄榄叶的化学成分研究

  荣,梁敬钰*,卢海英,杨  洋,刘 

(中国药科大学天然药物化学教研室,江苏南京210009



摘 要:对橄榄科橄榄属青橄榄树叶子的化学成分进行了研究。从乙酸乙酯萃取部位分得8个化合物,经理化及光谱方法鉴定分别为:没食子酸乙酯(Ⅰ)、东莨菪素(Ⅱ)、没食子酸(Ⅲ)、穗花杉双黄酮(Ⅳ)、肌醇(Ⅴ)、槲皮素(Ⅵ)、β-谷甾醇(Ⅶ)、4,5-去氢诃子裂酸三乙酯(Ⅷ)。其中化合物Ⅷ为新化合物,化合物Ⅴ、Ⅵ为首次从该属植物中得到,化合物Ⅳ、Ⅶ为首次从该植物中得到。

关键词:青橄榄树;4,5-去氢诃子裂酸三乙酯

中图分类号:TQ91   文献标识码:A   文章编号:0253-2417(2007)02-0045-04

 

Study  on  Chemical  Constituents  of  the Leaves  of  Canarium album(Lour.) Raeusch

CHEN Rong, LIANG Jing­yu, LU Hai­ying, YANG Yang, LIU Rui

(Department of Natural Medicinal Chemistry,China Pharmaceutical University,  Nanjing 210009,  China)

 

Abstract: Chemical constituents of the leaves of Canarium album (Lour.) Raeusch were studied.Eight compounds were isolated from ethylacetate extract of the leaf, and their structures were elucidated by various spectroscopic methods.They were identified as ethyl gallate(),scopoletin (),gallic acid (), amentoflavone (),myo­inositol(),quercetin (),β­sitosterol() and 4,5­didehydro­chebulic acid triethyl ester(). Compound is a novel compound and compounds and were obtained from this genus of plant for the first time. Compounds and were isolated from this plant for the first time.

Key words:Canarium album (Lour.) Raeusch;4,5­didehydro­chebulic acid triethyl ester

蓝花楹木质素-碳水化合物复合体在硫酸盐法蒸煮过程中的变化

周 燕12,谢益民1*,甘定能3,杨志勇12,王鹏4

1.山东轻工业学院制浆造纸工程省级重点学科,山东长清250353 2.潍坊科技职业学院化学工程学院,山东寿光262700 3.湖南岳阳纸业股份有限公司,湖南岳阳 4140024.华南理工大学制浆造纸工程国家重点实验室,广东广州510640

 

摘 要:以蓝花楹为原料提取木质素-碳水化合物复合体(LCC),并对LCC的结构进行分析,同时模拟硫酸盐法蒸煮过程,采用蒸煮的方法对LCC进行处理,并对处理后的产物进行红外光谱和核磁共振分析,研究蓝花楹LCC的结构变化,探讨其在硫酸盐法蒸煮过程中LCC的形成和降解情况。研究发现:蓝花楹LCC中的碳水化合物在蒸煮过程中非常不稳定,大部分发生降解,而蒸煮产物中含有对碱稳定的LCC结构,也含有新形成的LCC结构,这种新形成的LCC5-5缩合型木质素结构与木聚糖形成的以化学键连接的LCC结构,且其对碱也非常稳定。

关键词:木质素-碳水化合物复合体;硫酸盐法蒸煮;碳水化合物;蓝花楹

中图分类号:TQ91;TS711O636.2  文献标识码:A   文章编号:0253-2417(2007)02-0049-04

 

Change of Lignin­carbohydrate Complexes in Jacaranda copaia Aubl.D.Don. during Kraft Cooking

ZHOU Yan1,2, XIE Yi­min1, GAN Ding­neng3YANG Zhi­yong1,2WANG Peng4

(1.Shandong Key Lab. of Pulp and Paper Engineering,Shandong Institute of Light Industry, Changqing 250353, China;2.Weifang Science and Technology Vocational College, Shouguang 262700, China;3.Hunan Yueyang Paper Co.Ltd, Yueyang 414002, China; 4.State Key Lab. of Pulp and Paper Engineering,South China University of Technology, Guangzhou 510640, China)

 

Abstract: Lignin­carbohydrate complexes(LCC)from Jacaranda copaia Aubl.D.Don. was prepared. In order to research the degradation of LCC during cooking, LCC was treated by kraft method. The combination of infrared spectra analysis and 13C NMR was used to identify LCC formed during kraft cooking.The research indicated that carbohydrates in LCC were unstable and most of them were cleaved during kraft cooking. There were undegraded LCC and newly formed LCC structures after kraft cooking. The structure of  newly formed LCC was from  lignin structure and xylan, such as 5­5 lignin structure, which were connected with benzyl ether linkage. The newly formed LCC were stable in alkaline solution.

Key words:lignin­carbohydrate complexes;kraft cooking;carbohydrate;Jacaranda copaia Aubl.D.Don.

 

 

 

 

亚甲基蓝吸附值用活性炭标准样品的研制

戴伟娣, 孙康, 常 侠, 童娅娟, 张燕萍, 孙云娟

(中国林业科学研究院林产化学工业研究所;国家林业局林产化学工程

重点开放性实验室,江苏南京210042

 

摘 要:制备活性炭吸附性能标准样品,对于规范产品应用市场,减少应用和生产企业的产品性能测定误差,尤其对于提高和确定活性炭的质量检测水平和产品仲裁均有积极作用。本文主要论述了亚甲基蓝吸附值用活性炭标准样品的研究过程,以及性能指标的可信性和稳定性研究。研制结果表明,该活性炭标准样品的均匀性、稳定性良好。该批次的标准活性炭的定值为:亚甲基蓝吸附值的标准值为 225 mg/g(滤液吸光度0.053);滤液吸光度的标准不确定度(U0.009;扩展不确定度(置信水平为95 %0.018;采用每袋5 g标准样品包装并密闭保存,15个月内标准样品质量稳定性好,对分析数据进行Grubbs检验,置信度在95 %以上。

关键词:活性炭;标准样品;亚甲基蓝吸附值;木屑

中图分类号:TQ424.1   文献标识码:A   文章编号:0253-2417(2007)02-0053-04

 

Research on Preparation of Standard Reference Material of  Activated Carbon  for Methylene Blue Adsorption

DAI Wei­di, SUN Kang, CHANG Xia, TONG Ya­juan, ZHANG Yan­ping, SUN Yun­juan

(Institute of Chemical Industry of Forest Products,CAF; Key and Open Lab.on

Forest Chemical Engineering,SFA, Nanjing 210042, China)

 

Abstract: The preparation of standard reference material of activated carbon has positive significances of standardizing markets, application and reducing  measurement error during appliance and production, especially enhancing testing level and confirming products arbitration. The researches  on preparation of standard reference material of activated carbon for adsorption of methylene blue, its homogeneity and stability are described. The results show that homogeneity and stability of this activated carbon standard reference material are very good. The certified values of this batch of activated carbon standard reference material are: standard value of methylene blue adsorption is 225 mg/g (filter liquor absorbance 0.053); the filter liquor standard uncertainty U is 0.009; extended uncertainty (confidence level is 95 %) is 0.018. Per 5 g of standard reference material is packed in a bag, closely for storage. Within 15 months, the stability of standard reference material is good. Through Grubbs proof, the confidence level is above 95 %.

Key words:activated carbon;standard reference material;methylene blue adsorption;

chip

 

 

 

 

糠醇蒸汽沉积聚合法制备有序中孔炭分子筛

黄 莉1,王重庆1,李 青1,张利雄1*,陆现彩2

(1. 南京工业大学化学化工学院;江苏省材料化学工程重点实验室,江苏南京2100092. 南京大学地球科学系,江苏南京210093)

 

摘 要:以纯硅MCM-48为模板、对甲苯磺酸为催化剂、糠醇为碳源通过蒸汽沉积聚合制备了高度有序的中孔炭分子筛。先用真空浸渍法将酸性催化剂对甲苯磺酸引入模板MCM-48孔道内, 然后采用蒸汽气相沉积法将糠醇引入模板孔道内并聚合。研究发现,浸渍催化剂后的模板最好用乙醇冲洗以去除负载于模板表面的多余催化剂,适宜的乙醇冲洗量为每克模板10 mL;引入蒸汽沉积时间以12 h为宜;产物用XRDN2吸附等进行了表征,表明所制得的中孔炭具有规整的三维孔道结构和多重中孔分布。

关键词:中孔炭分子筛;糠醇;蒸汽沉积;MCM-48

中图分类号:TQ175.714   文献标识码:A   文章编号:0253-2417(2007)02-0057-05

 

Synthesis of Ordered Mesoporous Carbon from Furfuryl Alcohol by Vapor Deposition Polymerization Method

HUANG Li1, WANG Chong­qing1, LI Qing1, ZHANG Li­xiong1, LU Xian­cai2

(1.College of Chemistry and Chemical Engineering,Nanjing University of Technology;Key Lab of Materialsoriented Chemical Engineering of Jiangsu Province, Nanjing 210009, China; 2.State Key Laboratory of Mineral Deposit Research,Department of Earth Sciences,Nanjing University, Nanjing 210093, China)

 

Abstract: Ordered mesoporous carbon was successfully synthesized using siliceous MCM­48 as template, p­toluenesulfonic acid (PTSA) as catalyst, and furfuryl alcohol as carbon source by vapor depositon polymerization method. First, PTSA was introduced into the pores of MCM­48 by vacuum infiltration, then  MCM­48 was allowed to contact with the vapor of furfural alcohol at 90 . The suitable reaction time was about 12 h. It was found that MCM­48,after impregnated with PTSA,had better been washed with certain amount of ethanol to remove extra PTSA.The proper amount of ethanol was 10 mL/g MCM­48. The obtained mesoporous carbon was characterized by XRD and N2 adsorption. XRD result showed the ordered three­dimensional channel structure and multiple mesoporous distribution of this carbon.

Key words:mesoporous carbo, n;furfuryl alcohol;vapor deposition polymerization;

MCM­48

 

 

 

黄檗主要药用成分的分布规律

秦彦杰1,2,王  1,阎秀峰1*

1. 东北林业大学生命科学学院,黑龙江哈尔滨1500402. 河北省地理科学研究所,河北石家庄050011

 

摘 要:对黄檗主要药用成分小檗碱、掌叶防己碱和药根碱在成树、幼树中的分布和季节变化进行了系统的研究。结果表明:黄檗树干韧皮部中3种生物碱含量均随着树干位置增高而降低,成树在地面至1.5 m高度内随位置增高而急剧下降,超过1.5 m后趋于平稳,而幼树随位置增高近线性下降,幼树近地面 20 cm茎段韧皮部中的小檗碱含量相当于成树;黄檗成树韧皮部中3种生物碱含量的季节变化不明显,而生长2年的黄檗幼树韧皮部中则有明显的季节变化,根是7月含量较高,茎是6月含量较高。

关键词:黄檗;药用成分;部位差异;季节变化

中图分类号:TQ91;S792.31   文献标识码:A   文章编号:0253-2417(2007)02-0062-05

 

Distribution Pattern of Principal Medicinal Constituents in Amur Corktree

QIN Yan­jie1,2, WANG Yang1, YAN Xiu­feng1

(1.College of Life Sciences,Northeast Forestry University, Harbin 150010, China;2.Geographical Science Institute of Hebei, Shijiazhuang 050011, China)

 

Abstract: Seasonal variation and distribution of principal medicinal constituents,namely berberine, palmatine and jatrorrhizine in mature trees and saplings of amur corktree ( Phellodendron amurense Rupr.) were studied. In mature trees, alkaloids were decreased from base to the apex in the phloem, sharply dropped down at the height of 1.5 m from the base, then turned steady above the height of 1.5 m; whereas in saplings, alkaloids levels declined linearly with the increased height from the base.The alkaloids content at the height of 20 cm from the base was equivalent to that at the height of 1.5 m in mature tree. In contrast to an unobvious seasonal variation of alkaloids content in mature tree, alkaloids content in two year saplings changed remarkably, the highest contents were showed in July in roots and in June in the stem.

Key words: amur corktree (Phellodendron amurense Rupr.)medicinal constituentspositional differenceseasonal variation

 

 

 

纳米纤维素/聚乙二醇固-固相变材料的制备及其储能性能的研究

原小平12,丁恩勇1*

1. 中国科学院广州化学研究所纤维素化学重点实验室,广东广州5106502. 中国科学院研究生院,北京100039

 

摘 要:介绍了以纳米纤维素(NCC)为骨架材料、聚乙二醇(PEG)为相变储能功能基,采用化学接枝的方法制备一种NCC/PEG-固相变材料。并分别用IRDSC以及TGA等技术手段对其储能性能进行表征。结果表明,以纳米纤维素为骨架材料制备的固-固相变材料具有更高的相变焓,所得的相变材料具有更好的储能效率,其相变焓最大可达103.8 J/g

关键词:纳米纤维素;固-固相变材料;化学接枝;储能效率

中图分类号:TQ352Q539.2   文献标识码:A   文章编号:0253-2417(2007)02-0067-04

 

Preparation of Nanocrystalline Cellulose/Polyethylene Glycol Solidsolid Phase Transition Material and  Its Energy Storage Characteristics

YUAN Xiaoping1,2,  DING Enyong1

(1. Key Laboratory of Cellulose and Lignocellulosics Chemistry,Guangzhou Institute of Chemistry,Chinese Academy of Sciences, Guangzhou 510650,  China; 2. Graduate School of the Chinese Academy of Sciences, Beijing 100039, China)

 

Abstract: A new kind of solid­solid phase transition material (PCM) was prepared. The material is composed of two parts,in which polyethylene glycol (PEG) is the functional surface for energy storage and nano­crystalline cellulose (NCC) is the skeleton. The flexible polymer PEG was grafted onto the surface of the rigid polymer NCC through covalent bonds. Furthermore energy storage properties of  PCM were studied by means of FT­IR, DSC, TGA,etc..Results show that PCM possesses high enthalpy of phase transition up to 103.8 J/g, and high efficiency of energy storage.

Key words:nano­crystalline cellulose;solid­solid phase transition material;

chemical grafting;efficiency of energy storage

 

 

 

核桃叶中抗植物病毒活性物质提取条件的研究

翟梅枝,景炳年,贾彩霞,刘朝斌

( 西北农林科技大学林学院,陕西杨凌712100



摘 要:以不同溶剂和方法对核桃叶进行了抗植物病毒物质的提取和活性测定。结果表明:提取物的抗病毒活性因提取溶剂和提取方法的不同而异。以体积分数95 %乙醇为提取溶剂,冷浸提取物在质量浓度10g/L时,对烟草花叶病毒(TMV) 的抑制率最高,为100 %。采用冷浸提取时,核桃叶中抗TMV活性物质提取的优化条件是:以体积分数95 %乙醇为提取溶剂,料液比110(gmL),提取18 h,得率 21.42 %。质量浓度5g/L的提取物对TMV侵染心叶烟的抑制率为100 %。该提取物的乙酸乙酯萃取物经多次层析分离和纯化得到黄酮类化合物A,质量浓度0.5g/L的化合物ATMV侵染心叶烟的抑制率达85.55 %,说明化合物A是乙酸乙酯萃取物中的主要抗病毒活性成分之一。

关键词:核桃;烟草花叶病毒;提取方法

中图分类号:TQ91   文献标识码:A   文章编号:0253-2417(2007)02-0071-05

 

Study on  Extraction Conditions of Active Antiviral Substance from Walnut Leaves

ZHAI Mei­zhi, JING Bing­nian, JIA Cai­xia, LIU Chao­bin

(College of Forestry,Northwest Agriculture and Forestry  University, Yangling 712100, China)

 

Abstract: Antiviral substances of walnut (Juglans regia L.) leaves were extracted by different solvents and methods, and their antiviral activities were determined. The results showed that antiviral activity is dissimilar based on extracts from walnut leaves with different solvent and methods.For cold­leached extract with 95 %ethanol, when concentration inoculated is 10g/L, inhibition rate on tobacco mosaic virus(TMV) of the extract was the best, 100 %; optimum extraction condition of this extract is: 95 % ethanol as solvent, ratio of material to solvent 110, soaking time 18 h, extraction rate  21.42 %. The inhibition rate of the extract on TMV infecting Nicotiana glutinosa is 100 % when concentration inoculated is 5g/L.Besides,an antiviral flavonoid A was isolated from ethyl acetate extract through column chromatography,thin layer chromatography and recrystallization.When its concentration inoculated is  0.5g/L, inhibition rate of this compound on TMV infecting N.glutinosa is 85.55 %. The result indicated that compound A is one of the main antiviral components in ethyl acetate extract.

Key words:walnut(Juglans regia L.);tobacco mosaic virus;extraction method

 

 

 

银杏叶生产饲料复合酶的固态发酵条件及产物分析

赵林果1,曹福亮2,喻 涛3,李同军3,汪贵斌2

1.南京林业大学化学工程学院,江苏南京210037; 2.南京林业大学森林资源与环境学院,江苏南京210037;  3. 南京福润德动物药业有限公司,江苏南京210003

 

摘 要:研究了以银杏叶为原料,黑曲霉为菌种生产饲料复合酶的固态发酵条件,分析了发酵产物中主要营养成分和活性成分的变化。结果表明,适宜的工艺参数为:浅盘发酵的料层厚度4 cm,初始含水率为64.3 %,培养基初始pH5.0,接种量 2.5 %,培养温度2830 ℃。银杏叶通过生物转化后营养丰富,生物活性增强。其中,粗蛋白、总氨基酸、必需氨基酸分别提高106.09 %69.26 %79.17 %;总黄酮提取率提高5.77 %;纤维素酶和半纤维素酶的活力分别达到11.83122.17U/g。同时,产品中还富含高活力的风味酶(β-葡萄糖苷酶),其活力为36.11U/g,该酶使产品的生物活性及香味得到了明显的改善。

关键词:复合酶;饲料添加剂;银杏叶;固态发酵;纤维素酶活

中图分类号:TQ91   文献标识码:A   文章编号:0253-2417(2007)02-0076-05

 

Conditions of Solid Fermentation of Ginkgo bilobaL. Leaves to Produce Forage Multienzyme and Analysis of the Product

ZHAO Lin­guo1, CAO Fu­liang2, YU Tao3, LI Tong­jun3, WANG Gui­bin2

(1. College of Chemical Engineering,Nanjing Forestry University, Nanjing 210037, China;2. College of Forest Resources and Environment,Nanjing Forestry University, Nanjing 210037, China;3. Nanjing Furunde Animal Pharmacy Limited Company, Nanjing 210037, China)

 

Abstract: The culture condition of solid fermentation of Ginkgo biloba L. leaves to produce forage multienzyme and the changes of main nutritional ingredients and functional ingredients of the fermented products were studied. The optimum culture conditions were: substrate thickness 4 cm in shallow tray fermentors; initial moisture content 64.3 %; inoculum dosage 2.5 %; initial pH value 5.0; incubation temperature 28-30 . The analysis of the fermented products showed that contents of crude protein, total amino acids, necessary amino acids were increased 106.09 %, 69.26 %and 79.17 %, respectivelythe extraction rate of flavonoids was improved by 5.77 %; cellulase and hemicellulase activities were 11.83U/g and 122.17U/g, respectively.Furthermore, the final product contained highly active β­glucosidase, with activity of 36.11U/g, which distinctly improved the function and fragrance of the product.

Key words:multienzyme;forage additive;Ginkgo biloba L. leaves;solid fermentation;

cellulase activity

 

 

 

兴安落叶松单宁含量的器官差异与季节变化

王文杰,祖元刚*,李雪莹

(东北林业大学森林生态学教育部重点实验室,黑龙江哈尔滨150040



摘 要:兴安落叶松是生产落叶松单宁的重要原材料,随着天保工程的实施,使得主要原料树皮供应紧张。通过20032004年的测定结果表明,除现用的树皮(8.8 %15.4 %)生产原料外,根系(约7.8 %)、树枝( 1.0 %7.0 %)甚至叶片(4.0 %8.0 %)都可以成为生产原料,而树干木质部含量过低( 0.6 %1.4 %)不宜成为生产原材料。不同季节单宁含量差异结果表明,秋季(910月)的落叶松单宁含量都显著高于其它季节,因此,原材料的收集应该在秋季。此外,叶片单宁含量与光照强度呈现显著正相关。

关键词:兴安落叶松;单宁;季节变化;器官差异

中图分类号:TQ943.2   文献标识码:A   文章编号:0253-2417(2007)02-0081-04

 

Seasonal Change and Organs Difference of Tannin Content in Larix gmelinii

WANG Wen­jie, ZU Yuan­gang, LI Xue­ying

(Key Laboratory of Forest Plant Ecology Ministry of Education of the Peoples Republic of China,Northeast Forestry University,  Harbin 150040, China)

 

Abstract: The main raw material for tannin related products is  Larix gmelinii (Rupr.)Rupr. in northeast China.However,bark materials are short of supply since the implementation of forest protection. The results in this study (carried out during 2003-2004) showed that roots (tannins about 7.8 %), branches (1.0 %-7.0 %) even leaves (4.0 %-8.0 %) can be used as raw materials beside bark (8.8 %-15.4 %) as the most popular raw materials.However, xylem in stem is not a suitable material because of the too low tannin content (0.6 %-1.4 %). The data of seasonal changes of tannin in different organs showed a general pattern, i.e. different organs in autumn (Sept. to Oct.) had significantly higher content of tannin compared to other seasons, indicating that autumn is the optimal time for material collection. Furthermore, tannin content in leaves is positively correlated with intensity of sunlight.

Key words:Larix gmelinii (Rupr.)Rupr.;tannins;seasonal changes;organs differences

 

 

 

绿原酸的提取及稀土配合物抗菌活性测定

罗 娟,李友凤,胡晓莲,潘 志,屈景年

(湖南科技大学化学化工学院,湖南湘潭411201



摘 要:以乙酸乙酯和0.05 mol/L HCl组成的混合溶液作萃取剂,从金银花中一步提取绿原酸。研究了乙酸乙酯体积分数、温度、浸取时间对提取绿原酸的影响。并用绿原酸与LaCl3·6H2O反应合成了绿原酸合镧(Ⅲ)配合物,通过元素分析、红外光谱、重分析和化学分析,确定配合物的组成为:[La(C16H17O9)3]·2H2O。测试了配体和配合物分别对革兰氏阴性菌(大肠杆菌)和革兰氏阳性菌(金黄色葡萄球菌)的抗菌活性。实验结果表明,提取绿原酸最佳实验条件是:温度65 ℃,乙酸乙酯体积分数80 %,浸取时间3 h。提取物相对原料量的质量分数为3.21 %,绿原酸的质量分数86.3 %;绿原酸抗金黄色葡萄球菌的活性比抗大肠杆菌强。配合物对大肠杆菌的抗菌活性比配体明显增强,但对金黄色葡萄球菌的抗菌活性反而比配体弱。

关键词:绿原酸;金银花;抗菌活性

中图分类号:TQ91   文献标识码:A   文章编号:0253-2417(2007)02-0085-04

 

Study on Extraction of Chlorogenic Acid and Determination of Antibacterial Activity of Its Rare­earth Complexes

LUO JuanLI You­fengHU Xiao­lianPAN Zhi, QU Jing­nian

(College of Chemistry and Chemical Engineering,Hunan University of Science and Technology, Xiangtan  411201, China)

 

Abstract: Chlorogenic acid is extracted from Lonicera japonica Thunb. directly with extractant which is composed of ethyl acetate and hydrochloric acid ( 0.05 mol/L), and the effects of volume fraction of ethyl acetate, temperature and leaching time on extraction are investigated. The complex of La3+ is synthesized by the reaction of chlorogenic acid with LaCl3·6H2O,and the confirmed complex structure is La(C16H17O9)3]·2H2O by elemental microanalysis,infrared spectroscopy(IR), and thermogravimetry analysis (TG). Moreover, the antibiotic activities of ligand and complex against Gram­negative bacteria and Gram­positive bacteria are also tested. The results show: that the optimum condition of extaction of chlorogenic acid is: temperature 65 , volume fraction of ethyl acetate 80 %, leaching time 3 h, mass ratio of extracting substances to lonicerae flos 3.21 %,and mass fraction of chlorogenic acid 86.3 %The antibacterial activity of chlorogenic acid against Staphylococcus aureus is stronger than  Escheria coli. The antibacterial activity of the complex against E. coli is evidently stronger than that of the ligand. In contrast, antibacterial activity of the complexes against S. aureus is weaker than that of the ligand.

Key words: chlorogenic acid;Lonicera japonica Thunb.;antibiotic activity

 

 

 

里氏木霉木聚糖酶降解粗碱木质素中木聚糖的研究

付强善, 姚春才*, 勇 强

(南京林业大学化学工程学院,江苏南京210037

 

摘 要:研究用里氏木霉木聚糖酶降解粗碱木质素中的木聚糖,得出了适宜的酶解条件:pH4.8、温度45 ℃、酶解时间4 h。还探讨了固形物浓度和酶用量对除糖率的影响。结果表明,随着固形物浓度的增加,除糖率逐渐降低;木聚糖酶用量越大,除糖率越高。

关键词:木聚糖酶;粗碱木质素;酶解;除糖率

中图分类号:TQ351.377Q556   文献标识码:A   文章编号:0253-2417(2007)02-0089-03

 

Enzymatic Hydrolysis of Xylan in Raw Alkaline Lignin by Xylanase from Trichoderma reesei

FU Qiang­shan YAO Chun­caiYONG Qiang

College of Chemical Engineering,Nanjing Forestry University, Nanjing 210037, China

 

Abstract: Enzymatic hydrolysis of xylan in raw alkaline lignin by xylanase from Trichoderma reesei was studied. The optimal hydrolysis conditions were determined as follows: pH value 4.8,temperature 45 , hydrolysis time 4 h. The effects of solid concentration and enzyme dosage on sugar removing rate were also investigated. Results showed that sugar removing rate decreases as solid concentration increases and that the higher the enzyme dosage, the larger is the sugar removing rate.

Key words:xylanaseraw alkaline ligninenzymatic hydrolysissugar removing rate

 

 

 

 

179种植物叶中β-胡萝卜素含量分析

郭圣茂1,2,赖晓莲1,邱业先3,彭 , 4,杜天真1*

(1.江西农业大学园林与艺术学院,江西南昌330045 2.北京林业大学资源与环境学院,北京100083 3.苏州科技学院生物系,江苏苏州2150094.江西师范大学生命科学学院,江西南昌330027)

 

摘 要:为探索新的植物β-胡萝卜素,采用纸层析法对分属52科的179种亚热带植物鲜叶中的β-胡萝卜素含量进行了分析。结果表明:β-胡萝卜素含量低于 20.0 mg/kg的植物有69种,介于20.050.0 mg/kg的植物有88种,高于50 mg/kg的植物22种;在52科植物中,竹亚科和壳斗科植物叶中β-胡萝卜素含量较高,其中含量最高的是板栗,为67.75 mg/kg,具有较高的研究和开发价值。

关键词:亚热带植物;β-胡萝卜素; 纸层析

中图分类号:TQ91   文献标识码:A   文章编号:0253-2417(2007)02-0092-05

 

Determination of β­carotene Contents in Leaves of 179 Plants

GUO Sheng­mao1,2, LAI Xiao­lian1, QIU Ye­xian3, PENG Ren4DU Tian­zhen1

(1.College of Landscape Architecture and Art,Jiangxi Agricultural University, Nanchang 330045, China;2. College of Resources and Environment,Beijing Forestry University, Beijing 100083, China3. Dept. of Biology,Suzhou Science and Technology University, Suzhou 215009, China;4. Life Science School,Jiangxi Normal University, Nanchang 330027, China)

 

Abstract: To explore new plantβ­carotene, the content of β­carotene in leaves of 179 species belonging to 52 families in subtropical China were determined by paper chromatography. In 69 species,β­carotene contents were less than 20.0 mg/kg. In 88 species,contents were 20.0-50.0 mg/kg. In 22 species, contents were higher than 50 mg/kg. The contents in families of Bambuseae and Fagaceae were higher than other families, in which the content of Castanea mollissima was the highest, which was 67.75 mg/kg, having high value of research and exploitation.

Key words:subtropics plant;β­carotene;paper chromatography

 

 

 

含氟脱氢枞胺Schiff 碱的合成及抑菌活性

饶小平,宋湛谦*,高 宏

(中国林业科学研究院林产化学工业研究所;国家林业局林产化学工程重点开放性实验室,江苏南京210042

 

摘 要:用直接缩合法合成了含氟的取代苯甲醛缩脱氢枞胺Schiff 碱,用IR1H NMR光谱确证其结构。对含氟Schiff 碱进行体外抑菌活性试验。结果表明,含氟的取代苯甲醛缩脱氢枞胺Schiff 碱对金黄色葡萄球菌和枯草芽孢杆菌等多种细菌有较强的抑制作用。对氟苯甲醛缩脱氢枞胺Schiff 碱对金黄色葡萄球菌以及枯草芽孢杆菌的抑制作用最强,抑菌圈直径分别达到1.651.30 cm;氟的引入对大肠杆菌无效,抑制能力反而降低。

关键词:取代苯甲醛缩脱氢枞胺;含氟Schiff 碱;抑菌活性

中图分类号:TQ423   文献标识码:A   文章编号:0253-2417(2007)02-0097-03

 

Synthesis and Antibacterial Activity of Fluorine­containing Schiff Bases Derived from Dehydroabietylamine

RAO Xiao­ping, SONG Zhan­qian, GAO Hong

(Institute of Chemical Industry of Forest Products,CAF;Key and Open Lab.on Forest Chemical Engineering,SFA, Nanjing 210042, China)

 

Abstract: Fluorine­containing substituted benzaldehyde semi­dehydroabietylamine Schiff bases were synthesized by direct condensation, and their structures were characterized by IR and 1H NMR spectroscopy. The antibacterial activities of fluorine­containing Schiff bases were tested by extracorporeal experiments.It has been found that fluorine­containing substituted benzaldehyde semi­dehydroabiety­

lamine Schiff bases displayed strong antibacterial activities against many kinds of bacteria such as Staphylococcus aureus and Bacillus subtilis.p­F­substituted benzaldehyde semi­dehydroabietylamine Schiff base has the strongest activity against S.aureus.and B.subtilis. The diameters of antibacterial rings reached 1.65 and 1.30 cm, respectively. The introduction of fluorine atom in Schiff base was ineffective against Escherichia coli, the activity was even reduced.

Key words:substituted benzaldehyde semi­dehydroabietylamine;fluorine­containing Schiff base;antibacterial activity

 

 

 

中压硅胶柱层析连续纯化茶叶中EGCGECG的研究

  1,高彦华1,祖元刚1*,祖述冲2

(1.东北林业大学植物药工程研究中心,黑龙江哈尔滨150040;2.东北林业大学职业技术学院,黑龙江哈尔滨150040



摘 要:采用一种连续中压硅胶柱层析分离高纯度表没食子儿茶素没食子酸酯(EGCG)及表儿茶素没食子酸酯(ECG,原料为含量高于98 %的茶多酚。连续中压柱层析分离工艺条件为: 160280μm硅胶为填充料,1 200 mm×80 mm的自制不锈钢中压层析柱,洗脱液为乙酸乙酯-石油醚-甲酸(体积比641),洗脱流速为30 mL/min,负载量为35 g/kg(以硅胶计,下同),可以得到纯度大于98 %EGCG产品(平均回收率为85.5 %)和98 %ECG产品(平均回收率均为80.3 %)。回收的洗脱剂先校正pH值,再经薄层层析校正后可重复使用。使用后的层析柱用乙酸乙酯再生,石油醚为平衡剂平衡,平衡后的层析柱可重复使用。

关键词:表没食子儿茶素没食子酸酯;表儿茶素没食子酸酯;硅胶;连续中压柱层析

中图分类号:TQ91;Q949.744   文献标识码:A   文章编号:0253-2417(2007)02-0100-05

 

Study on Successive Purification of Epigallocatechin Gallate and Epicatechin Gallate by Column Chromatography

YANG Lei1, GAO Yan­hua1, ZU Yuan­gang1, ZU Shu­chong2

(1.Engineering Research Center of Plant Medical,Northeast Forestry University, Harbin 150040, China2.Vocational and Technical College,Northeast Forestry University, Harbin 150040, China)

 

Abstract: A method is described for successive purification of epigallocatechin gallate (EGCG) and epicatechin gallate (ECG) by medium­pressure silica gel column chromatography. The raw material was 98 %tea polyphenols. The operating conditions of the chromatographic steps were investigated and optimized, using 1 200 mm×80 mm stainless steel column as chromatographic column. The optimum condition was as followed160-280μm silica gel as filling material, ethyl acetate­petroleum ether­formic acid 641 as eluting solvent, flowing rate 30 mL/min, loading amount 35 g/kg silica gel.The average yields of 98 % EGCG and 98 % ECG were 85.5 % and      80.3 %, respectively. A reclaimed eluting solvent can be used repeatedly,its pH value is first adjusted, and concentration ratio is then adjusted by TLC method. The chromatographic column which was regenerated by ethyl acetate, and equilibrated with petroleum, can be used repeatedly.

Key words:epigallocatechin gallate;epicatechin gallate;silica gel;successive medium­pressure column chromatography

 

 

 

不同品系万寿菊花中叶黄素和叶黄素酯含量的测定

李大婧1,2,刘春泉2*,方桂珍3

1.东北林业大学林学院食品科学与工程教研室,黑龙江哈尔滨1500402.江苏省农科院原子能农业利用研究所,江苏南京2100143.东北林业大学材料科学与工程学院,黑龙江哈尔滨150040

 

摘 要:采用反相高效液相色谱法测定不同颜色万寿菊花(包括花瓣和花萼)中叶黄素和叶黄素酯的含量。通过与叶黄素标准品比较,并利用相同色谱条件下的色谱图确定万寿菊花中含有叶黄素和6种叶黄素二酯,即月桂酸-肉豆蔻酸酯、二肉豆蔻酸酯、肉豆蔻酸-棕榈酸酯、二棕榈酸酯、棕榈酸-硬脂酸酯及二硬脂酸酯。不同颜色万寿菊花中叶黄素和叶黄素酯的含量差别较大,黄绿色花色素含量为0.024 %,橙色花色素含量高达1.148 %(均以干花粉计),颜色越深,叶黄素酯含量越高。万寿菊花的色素含量与脂肪含量呈明显正相关(R2=0.974)。

关键词:万寿菊花;叶黄素;叶黄素酯;高效液相色谱

中图分类号:TQ91   文献标识码:A   文章编号:0253-2417(2007)02-0105-04

 

Determination of Contents of Lutein and Lutein Esters in Marigold Flowers(Tagetes erecta Linn.)

LI Da­jing1,2, LIU Chun­quan2, FANG Gui­zhen3

(1. Food Sciences and Engineering Department,College of Forestry,Northeast Forestry University, Harbin 150040, China;2.Institute of Application in Atomic Energy,Jiangsu Academy of Agricultural Sciences, Nanjing 210014,  China;3.College of Material Science and Engineering,Northeast Forestry University, Harbin 150040, China)

 

Abstract: Contents of lutein and lutein fatty acid esters in flower­heads (petals and calyces) of different colors of marigold were evaluated by high performance liquid chromatography. A typical chromatographic profile of pigments was characterized by the simultaneous presence of lutein and lutein esters  with standard samples of lutein. Six lutein esters from orange marigold flower, consisted of lutein laurate­myristate,dimyristate,myristate­palmitate, dipalmitate, palmitate­stea­

rate, and distearate diesters, were confirmed. The total contents of pigments in dry marigold flower flour varied from 0.024 % in greenish yellow flowers to 1.148 % in deep orange flowers. Differences in petal color were well related to the pigment content. Furthermore, a positive correlation between pigment concentration and fat content in marigold flower was found (R2=0.974).

Key words:marigold flowers(Tagetes erecta Linn.);lutein;lutein esters;HPLC

 

 

 

过渡金属樟脑磺酸盐的制备和表征

苏婷婷,姜 恒*,宫 红

(辽宁石油化工大学 石油化工学院,辽宁抚顺113001)

 

摘 要:合成了一系列过渡金属(锌、铜、镍、锰、钴和镉)樟脑磺酸盐,并用红外光谱仪和热重分析对其进行了表征。热重分析研究表明,所合成的几种过渡金属樟脑磺酸盐均含6个结晶水,并讨论了其无水化合物的热稳定性,其次序为:Cu(C10H15O4S)2<Co(C10H15O4S)2, Zn(C10H15O4S)2<Ni(C10H15O4S)2<Cd(C10H15O4S)2<Mn(C10H15O4S)2。并通过多种手段详细分析了空气气氛下各种盐的最终分解产物。

关键词:樟脑磺酸盐;热重分析

中图分类号:TQ351   文献标识码:A   文章编号:0253-2417(2007)02-0109-05

 

Preparation and Characterization of Transition Metal Camphorsulfonates

SU Ting­ting, JIANG Heng, GONG Hong

(College of Petrochemical Engineering,Liaoning University of Petroleum & Chemical Technology, Fushun 113001, China)

 

Abstract: A series of transition metal (Zn, Cu, Ni, Mn, Co and Cd) camphorsulfonates were synthesized. The composition and properties of these complexes are characterized by FT­IR spectroscopy and thermogravimetric analysis (TGA). As shown in TGA results, all these transition metal camphorsulfonates contain six water molecules. Thermal stabilities of anhydrous compounds were discussed in the order of:  Cu(C10H15O4S)2<Co(C10H15O4S)2<Zn(C10H15O4S)2<Ni(C10H15O4S)2<Cd(C10H15O4S)2<Mn(C10H15O4S)2. The end thermal decomposition products in air atmosphere were studied by various methods.

Key words:camphorsulfonates;thermogravimetric analysis

 

 

均相体系中β-蒎烯氧化制备诺蒎酸

马世营1,2,沈敏敏1,哈成勇1*

1.中国科学院广州化学研究所;纤维素化学重点实验室,广东广州510650;

2.中国科学院研究生院,北京100039



摘 要:利用水和叔丁醇的混合溶液作为反应的溶剂,用高锰酸钾氧化β-蒎烯制备诺蒎酸,考察了叔丁醇含量、高锰酸钾和碱用量以及温度对产物收率的影响。最佳反应条件:反应温度1525 ℃,β-蒎烯、KMnO4NaOH物质的量的比为131.5,用30 %的叔丁醇水溶液做溶剂,诺蒎酸的收率(质量分数)在70.0 %以上。

关键词:β-蒎烯;诺蒎酸;叔丁醇

中图分类号:TQ351.4   文献标识码:A   文章编号:0253-2417(2007)02-0114-03

 

Preparation of Nopinic Acid from β­pinene in Homogeneous System

MA Shi­ying1,2,  SHEN Min­min1,  HA Cheng­yong1

(1. Key Lab. of Cellulose and Lignocellulosics Chemistry,Guangzhou Institute of Chemistry,Chinese Academy of Sciences, Guangzhou 510650, China 2. Graduate School of Chinese Academy of Sciences, Beijing 100039, China)

 

Abstract: Nopinic acid was obtained from β­pinene oxidated by potassium permangate in the mixed solvent of tert­butanol and water. The effects of dosages of potassium permangated,tert­butanol,sodium hydroxide and temperature on yield were investigated.The optimum reaction condition was as follows:nβ­pinene)∶nKMnO4)∶nNaOH131.5,m(water)m(tert­butanol )73 and reaction temperature 15-25 .The yield of nopinic acid reached over 70.0 %.

Key words:β­pinene;nopinic acid;tert­butanol

 

快速搅拌法室温浸提印楝油和印楝素

李晓升12,赵吉寿2,王有琼1,马李一1,段琼芬1*

(1. 中国林业科学研究院资源昆虫研究所,云南昆明650224;

2. 云南民族大学化学与生物技术学院,云南昆明650031)

 

摘 要:在室温下用间歇式快速搅拌法从印楝种仁中浸提印楝油和印楝素。讨论了料液比以及浸提时间对得率的影响。结果表明:印楝种仁300 g,以750 mL石油醚做溶剂,在快速搅拌条件下浸提 21 min时印楝油得率最高;将300 g去油后的印楝种仁以900 mL甲醇做溶剂,在快速搅拌下浸提 21 min时印楝素得率最高。由此得出,快速搅拌法浸提印楝油的最佳条件是:溶剂石油醚、料液比12.5gmL,下同)、时间每次7 min、浸提3次,出油率30.4 %;快速搅拌法浸提印楝素的最佳条件是:溶剂为甲醇、料液比13、时间每次7 min、浸提3次,印楝素A的得率为0.438 %,印楝素B的得率为0.142 %

关键词:搅拌浸提;印楝油;印楝素

中图分类号:TQ91   文献标识码:A   文章编号:0253-2417(2007)02-0117-03

 

Rapid­agitation Extraction of Neem Oil and Azadirachtin at Room Temperature

LI Xiao­sheng1,2, ZHAO Ji­shou2, WANG You­qiong1, MA Li­yi1, DUAN Qiong­fen1

(1.Research Institute of Resources Insects,Chinese Academy of Forestry, Kunming 650224, China;2.Department of Chemistry and Biology,Yunnan Institute for Nationalities, Kunming 650031, China)

 

Abstract: Neem oil and azadirachtin were extracted batchwisely from neem seeds under rapid agitation at room temperature. The effects of solvent, components ratio and extraction time on the yield of neem oil and azadirachtin were discussed. The yield of neem oil was the highest under the condition as follows: 300 g neem seeds were rapidly agitated for 21 min in 750 mL petroleum ether.The highest yield of azadirachtin was obtained when  300 g skimmed neem seeds were rapidly agitated for 21 min in 900 mL methanol. The optimized condition of rapid agitation extraction of neem oil was:petroleum ether solvent, components ratio 12.5gmL, extraction time 7 min every time, for 3 times. The oil yield was 30.4 %. The optimized condition of rapid agitation extracion of azadirachtin was:methanol solvent, components ratio 13gmL, extraction time 7 min every time, for 3 times. The yields of azadirachtin A and azadirachtin B were  0.438 %and  0.142 %,respectively.

Key words:agitation extraction;neem oil;azadirachtin

 

 

 

K-卡拉胶与纳米微晶纤维素凝胶化的研究

郭 瑞1,2,丁恩勇13*

(1.中国科学院广州化学研究所;纤维素化学重点实验室,广东广州510650;

2. 中国科学院研究生院,北京100039;

3. 华南理工大学材料科学与工程学院,广东广州510641



摘 要:K-卡拉胶和纳米微晶纤维素(CNC)共混时可以得到凝胶多糖。多糖总质量分数为1 %,K-卡拉胶与纳米微晶纤维素的比例为91时,可达到协同相互作用的最大值。研究了pH值和体系盐离子浓度对凝胶强度的影响,并通过FT-IR光谱和Raman光谱对这两种多糖之间的相互作用机理进行了初步的探讨。

关键词:K-卡拉胶;纳米微晶纤维素;凝胶化

中图分类号:TQ351.47;O636   文献标识码:A   文章编号:0253-2417(2007)02-0120-03

 

Study on Gelation of K­carrageenan with Cellulose Nanocrystals

GUO Rui1,2DING En­yong1,3

(1.Key Lab.of Cellulose and Lignocellulosics Chemistry,Guangzhou Institute of Chemistry,Chinese Academy of Sciences,Guangzhou 510650, China 2.Graduate School of Chinese Academy of Sciences, Beijing 100039, China;3.College of Materials Science and Engineering,South China University of Technology, Guangzhou 510641, China)

 

Abstract: Mixing of K­carrageenan with cellulose nanocrystals (CNC) can form gel. A maximum synergistic interaction occurred when the mixed ratio of K­carrageenan and cellulose nanocrystals(CNC) was 91 at total mass fraction 1 % polysaccharide concentration. Effects of pH value and salt ion concentration on gel strength were studied. Interaction among molecules of these two polysaccharides was also investigated by FT­IR and Raman spectrometry.

Key words:K­carrageenancellulose nanocrystalsgelation

 

 

两性壳聚糖的制备及产物结构表征

蔡照胜12,宋湛谦1*,杨春生2,王锦堂3,许 琦2

1.中国林业科学研究院林产化学工业研究所;国家林业局林产化学工程重点开放性实验室,江苏南京210042 2.盐城工学院化学与生物工程学院,江苏盐城224003;3.南京工业大学理学院,江苏南京210009)

 

摘 要:以脱乙酰度大于90 %的壳聚糖(CTS)为原料,异丙醇为溶剂,ω(NaOH)40.0 %的碱液为催化剂,氯乙酸为羧甲基化试剂,NaOHCTS、氯乙酸的质量比为1.01.01.25、反应温度50.0 ℃、反应时间7.0 h的条件下制备了羧甲基壳聚糖(CM-CTS);以3--2-羟丙基三甲基氯化铵(CTA)为改性剂,NaOHCM-CTSCTA的质量比为1.02.03.0、反应温度60.0 ℃、反应时间10.0 h,制得CTA季铵化羧甲基壳聚糖(CTA-CMCTS)。IR1H NMR的结果表明,CTA-CMCTS为一既有季铵基团又有羧甲基的两性壳聚糖衍生物。以CTA-CMCTS为絮凝剂处理含Cd2+或含Cr6+模拟废水时,Cd2+Cr6+ 的最大絮凝去除率分别可达99.7 %94.4 %

关键词:羧甲基壳聚糖;3--2-羟丙基三甲基氯化铵;接枝试剂;两性壳聚糖;絮凝剂

中图分类号:TQ91O636.1   文献标识码:A   文章编号:0253-2417(2007)02-0123-04

 

Preparation of Amphoteric Chitosan and Characterization of Its Structure

CAI Zhao­sheng1,2, SONG Zhan­qian1, YANG Chun­sheng2, WANG Jin­tang3, XU Qi2

 (1.Institute of Chemical Industry of Forest Products,CAF;Key and Open Lab. on Forest Chemical Engineering,SFA, Nanjing 210042, China 2.Department of Chemical and Biological Engineering,Yancheng Institute of Technology,Yancheng 224003, China; 3.School of Science,Nanjing University of Technology, Nanjing 210009,  China)

 

Abstract: Using 2­propanol as solvent,ω(NaOH)40.0 %aqueous solution as catalyst, m(NaOH)m(CTS)m(ClCH2CO2H)1.01.01.25, reaction temperature 50.0 reaction time 7.0 h and ClCH2CO2H as carboxymethylating agent, carboxymethyl chitosan (CM­CTS) was prepared from chitosan, with a degree of deacetylation about 90 %.Then CM­CTS was modified with 3­chloro­2­hydroxypropyl trimethylammonium chloride (CTA) as grafting agent under conditions of m(NaOH)m(CM­CTS)m(CTA)1.02.03.0, reaction temperature 60.0 and reaction time 10.0 h. The product was characterized by IR and 1H NMR. The results indicated it to be an amphoteric derivative of chitosan. The simulated waste water containing Cd2+ or Cr6+ was treated with CTA­CMCTS as flocculating agent. The removal ratio of Cd2+ and Cr6+may reach 99.7 % and 94.4 %, respectively.

Key words: carboxymethyl chitosan;3­chloro­2­hydroxypropyl trimethyl­ammonium chloride;grafting agent;amphoteric chitosan;flocculant

 
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