Studies on the Interactions between Bioactive Peroxovanadium Complexes Bearing Organic Ligands and Histidine

在合成和表征了 4种具有较强生物活性双过氧钒配合物K3 [VO(O2 ) 2 (ox) ]·2H2 O ,Na[VO(O2 ) 2 (bipy) ]·5H2 O ,K[VO(O2 ) 2 (phen) ]·3H2 O和K2 [VO(O2 ) 2 (pic) ]·2H2 O [分别缩写为pV(ox) ,pV(bipy) ,pV(phen)和pV(pic) ,其中ox为草酸根 ,bipy为 2 ,2′ 联吡啶 ,phen为邻菲咯啉 ,pic为 2 羧酸吡啶负离子 ]的基础上 ,利用多种NMR技术和电喷雾质谱 (ESI MS)研究了这 4种含有机配体双过氧钒配合物与组氨酸 (His)在溶液中的相互作用以及反应物浓度、时间、pH等对相互作用体系的影响 .51VNMR跟踪监测的结果表明 :双过氧钒配合物pV(ox)和pV(pic)与His在中性水溶液中存在强配位相互作用 ,而pV(bipy)和pV(phen)与His在中性水溶液中无明显作用 .我们还利用谱学方法确定了pV(ox)和His相互作用后所生成产物是pV(ox)分别与His咪唑基上的 3 N和 1 N配位的一对异构体. 　In order to explore the structure2activity relationship and molecular mechanism of the specific recognition between peroxovanadium (pV) complexes bearing organic ligands and the target enzymes of tyrosine phosphatase , several NMR techniques and ESI2MS were used to study the interactions of four pV complexes {pV(ox) , pV ( bipy) , pV (phen) and pV (pic) , where pV = [VO (O2 ) 2L ] n - , in which L = oxalic acid dianion (ox) , bipyridine (bipy) , 1 ,102phenanthroline (phen) , and pyridine222carboxylic acid (pic) } towards histidine. Strong coordination interactions between imidazole of histidine and vanadium of pV(ox) or pV(pic) were observed in neutral solution , while there are not obvious interactions between histidine and pV(bipy) or pV(phen) . All 13C and 1H NMR signals of 1∶1 stoichiometric mixture of pV(ox) and histidine were assigned. Spectroscopic studies demonstrated that new complexes in the mixture of pV(ox) and histidine are a pair of isomers in which the vanadium in pV(ox) binding to the 32N and 12N of the imidazole ring. Moreover , the results of effective factors on the interaction system indicated that the new isomers were stable under the condition of physiological pH and the structure2activity relationship of these pV complexes may be relevant to their specific recognition towards histidine residues in tyrosine phosphatase.国家自然科学基金 (Nos.2 0 172 0 42 ,2 9832 0 2 0 )资助项

~(51)V NMR监测[VS_4Cu_n](n≤6)簇合物自兜反应过程

采用　51VNMR监测在核磁管内模拟 (NH4 ) 3VS4 /Et4 NBr/CuBr/PPh3体系在CH2 Cl2 中的反应过程 ,研究了反应条件如反应物不同配比对生成各种 [VS4 Cun](n≤ 6)簇合物的影响 ,提供了该反应体系在CH2 Cl2 溶液中成簇过程的一些信息 .该方法不仅可用来研究反应机理 ,而且可用于指导一些条件难以确定 (溶剂、温度、酸碱度等 )的簇合物如低核数及更高核数V Cu S簇合物的合

Studies on the interactions between bioactive peroxovanadium complexes bearing organic ligands and histidine

In order to explore the structure-activity relationship and molecular mechanism of the specific recognition between peroxovanadium. (pV) complexes bearing organic ligands and the target enzymes of tyrosine phosphatase, several NMR techniques and ESI-MS were used to study the interactions of four pV complexes {pV(ox), pV(bipy), pV(phen) and pV(pic), where pV=[VO(O-2)(2)L](n-), in which L=oxalic acid dianion (ox), bipyridine (bipy), 1, 10-phenanthroline (phen), and pyridine-2-carboxylic acid (pic)} towards histidine, Strong coordination interactions between imidazole of histidine and vanadium of pV(ox) or pV(pic) were observed in neutral solution, while there are not obvious interactions between histidine and pV(bipy) or pV (phen). All C-13 and H-1 NMR signals of 1:1 stoichiometric mixture of pV (ox) and histidine were assigned. Spectroscopic studies demonstrated that new complexes in the mixture of pV (ox) and histidine are a pair of isomers in which the vanadium in pV(ox) binding to the 3-N and 1-N of the imidazole ring. Moreover, the results of effective factors on the interaction system indicated that the new isomers were stable under the condition of physiological pH and the structure-activity relationship of these pV complexes may be relevant to their specific recognition towards histidine residues in tyrosine phosphatase

Studies on Valuable and Rare Chinese Herbs Anoectochilu s roxburghii by DNA Fingerprintings Using RAPD

王其新 男, 1 9 7 3 年毕业于中山大学药用植物学专业。现任湛江市药品检验所中药室主任, 主任中药师。擅长生药学、中药鉴定学和植物化学,连续参加三版中国药典部分药品标准的起草和修订工作, 对草豆范的薄层色谱鉴别进行了系统的研究。所建立的薄层色谱法被中国药典采用。编著著作1 本, 获广东药学院科技进步二等奖1 项, 发表科学论文28 篇, 取得“ 壮骨口服液” 发明专利1 项。为了鉴别金线莲的品种，探索同属植物之间的亲缘关系及同种 植物不同产地的遗传变异，并制定正品金线莲的 DNA 指纹图谱，采用随机扩增多态 DNA(RAPD)技术对兰科开唇兰属植物花叶开唇兰 Anoectochilus roxburghii(Wal-l.).Lindl.、台湾开唇兰 A.formosanus Hay. 进行了鉴定，结果选 择的 7 个引物对 3 个品种 共扩增出 98 个位点，其中 3 个引物为高特异性引物。结论 RAPD 技术不仅能鉴别种间差 异，而且能揭示同种不同产地植物的遗传变异。厦门市卫生局医学科学技术进步基金科研资助项

Effect of relieving fever and reducing plasmas glucose of 3 kinds of Digupi on albino rats

作者简介: 黄小红(1966- ) , 女, 讲师, 硕士. 研究方向: 动物生物化学.用 3种地骨皮 (枸杞根皮、宁夏枸杞根皮、北方枸杞根皮 )原生药总提取物灌喂大、小白鼠 ,测定它们对白鼠的解热和降血糖作用 .结果表明 :枸杞根皮和宁夏枸杞根皮对角叉菜胶致热的大白鼠有明显的解热作用 ;北方枸杞虽也有明显解热作用 ,但其作用强度弱于枸杞和宁夏枸杞 .3种枸杞根皮中仅枸杞根皮对四氧嘧啶小白鼠有明显降血糖作用 ,其余 2种地骨皮降血糖作用不甚明显

TLC-densitometric Determination of Scopoletin in Cortex Lycii

本文用双波长薄层扫描法首次测定了5种商品地骨皮药材中莨菪亭（SCOPOlETIn）的含量，以山西产地骨皮（lyCIuMCHInEnSEMIll.）的含量最高。The paper reported the content of scopoletin in 5 kinds of Cortex Lycii by TLC-densitometric determination For the First time.The results showed that the sample of the highest content was cortex of Lycium chinense From Shanxi province

福寿螺纤维素酶的开发与应用

以福寿螺内脏为材料 ,制备纤维素酶粉。测定各组分的酶活力分别为 :内切葡聚糖酶 2 0 .6 5万U/ g ;( β 葡萄糖苷酶 4.2 4万U/ g ;外切葡聚糖酶 0 .48万U/g ;酶粉的蛋白质含量为 37.6 9%、水分为 7.96 %、灰分为 1 .78%。以花生壳作为纤维素酶作用对象 ,测定酶促反应的最适pH为 5 .2 6 ,最适温度为 5 2℃。在 pH5 .2、40℃下 ,纤维素酶作用于花生壳生成葡萄糖 ,在 2h内葡萄糖的生成量与反应时间成正比关系 ,然后逐渐缓慢 ;随着酶浓度的增大 ,葡萄糖的量也呈直线上升 ,说明从福寿螺分离得到的纤维素酶能有效地水解花生壳转化为可被利用的葡萄糖

2D NMR Study on Solution Structure of Natural Product 3′-Methoxy Puerarin

【中文文摘】3′ 甲氧基葛根素是从常用中药野生葛根中分离提取出来的一种具有很强生物活性的异黄酮类化合物.该化合物含季碳较多,有些13CNMR的谱峰不易归属.本文利用包括氢检测异核多量子相干谱(HMQC)和氢检测远程异核多量子相干谱(HMBC)等多种二维核磁共振技术对该天然产物的13C和1HNMR谱峰进行了全归属.这些工作有助于利用二维核磁共振技术研究和确定含季碳较多的异黄酮类新化合物的结构和利用扩散相关的核磁共振新技术研究葛根的生理活性成份与靶分子相互作用. 【英文文摘】An active isoflavone compound 3′methoxy puerarin was isolated from puerarin lobate (willd). Several twodimensional NMR new techniques, including 1Hdetected heteronuclear multiplequantum coherence and 1Hdetected multiplebond heteronuclear multiplequantum coherence, were employed to completely assign all the protons and carbons of the compound. This work solves the assignments of uncertain C3 and C1′ NMR signals in the previous literature and will be helpful to study the structures of this kind of new isoflavone compounds by 2D NMR spectroscopy and bioactive compounds in puerarin lobate directly by diffusion2chemical shift 2D NMR.国家自然科学基金(20172042);; 国家中医药管理局与福建省卫生厅基金(2000 J P 40)资助项

乙二醇对长毛对虾酸性磷酸酶活力与构象的影响

应用荧光光谱、紫外差示光谱及园二色性光谱等生物物理技术研究长毛对虾酸性磷酸酶经乙二醇微扰后的分子构象变化情况，结果表明乙二醇对酶分子构象有显著的影响。酶的内源荧光强度随乙二醇浓度增大而增强，Ｔｙｒ、 Ｔｒｐ残基的微环境发生明显的变化；紫外差示光谱在 ２２０和 ２７５ｕｍ出现２个负峰，而 ２３６ｕｍ出现正峰， ２２０和２３６ ｕｍ的差吸收与酶分子主链去折叠有关，而 ２７５ ｕｍ主要与 Ｔｒｐ残基微环境变化有关；乙二醇变性后，酶的园二色性光谱变化说明酶分子二级结构也发生了明显的变化。比较酶在乙二醇溶液中失活与去折叠的关系，结果表明：酶在乙二醇溶液中的失活作用明显快于构象的变化，说明酶活性中心处于对变性剂乙二醇较为敏感的区域