聚[碳酸(亚丁酯-co-ε-己内酯)酯]的制备及其载药微球性能的研究

采用阴离子配位聚合方法, 合成了二氧化碳、1,2-环氧丁烷与ε-己内酯的三元共聚物: 聚[碳酸(亚丁酯-co-ε-己内酯)酯](PBCL). 并采用复相乳液(W/O/W)溶剂挥发法制备了包裹抗菌药物甲磺酸帕珠沙星的可降解微球. 对聚合物进行了FTIR, ¹H NMR, ¹³C NMR, DSC, TGA和WAXD等表征, 以及降解性能和载药微球特性的研究. 结果表明, PBCL热稳定性及降解性能优于聚碳酸亚丁酯(PBC). 所得PBCL微球球形规整、表面光滑. 大部分微球粒径在0.5～1 μm的范围内, 载药量和包封率分别达到38.21%和87.9%. 微球的体外释药性能研究在pH 7.4的磷酸缓冲溶液中进行, 释放21 d后, PBCL微球的累积释药量为84.74%, PBC微球的释药量仅为17.29%. 药物的体外释放行为符合Higuchi方程. PBCL载药微球具有长效缓释作用.     

多孔二氧化硅中Gd3+ → Eu3+的能量传递

通过水热反应法，获得了单掺和双掺Eu³⁺，Gd³⁺的多孔二氧化硅组装体，研究了掺杂体系的光谱特性，观察到Gd³⁺ → Eu³⁺的能量传递。分析了能量传递过程，探讨了在多孔二氧化硅中Gd³⁺→Eu³⁺的能量传递的机理，其机理主要为电偶极-电偶极相互作用。     

消旋的有机二磺酸三邻菲咯啉锌配合物(英)

Compound [Zn(phen)₃][BDA] (1) (BDA=6,6′-dibromo-2,2′-dimethoxy-1,1′-binaphthylene-4,4′-disulfonate, phen= 1,10-phenanthroline) composes of the anion part (racemic-(R,S)-6,6′-dibromo-2,2′-dimethoxy-1,1′-binaphthylene-4,4′-disulfonate ) and the cation part which consists of a racemic octahedrally coordinated zinc center defined six nitrogen atoms from three phen rings to form an inorganic chirality that can be resolution by chiral organic ligand, the 3D framework was formed through the strong H-bonding interaction between sulfonate and water. CCDC: 277924.     

Isolation and purification of flavonoid glycosides from Trollius ledebouri using high-speed counter-current chromatography by stepwise increasing the flow-rate of the mobile phase

Three flavonoid glycosides including orientin, vitexin, quercetin-3-O-neohesperidoside and one unknown compound were isolated and purified by high-speed counter-current chromatography (HSCCC) and semi-preparative HPLC from Trollius ledebouri Reichb., a traditional Chinese medicine. Preparative HSCCC with a two-phase solvent system composed of ethyl acetate-n-butanol-water (2:1:3, v/v/v) was successfully performed by increasing the flow-rate of the mobile phase from 1.5 to 2.5 ml/min after 190 min. Consequently, 95.8 mg orientin, 11.6 mg vitexin, 9.3 mg unknown compound with purities of over 97% and one partially purified peak fraction (contained quercetin-3-O-neohesperidoside at 85.1% purity) were obtained from 500 mg of the crude extract. Then the partially purified fraction was further purified by reversed-phase semi-preparative high-performance liquid chromatography. The structure identification of all pure fractions was carried out by UV, MS, 1H NMR and 13C NMR.     

咪唑类配体与双过氧钒配合物相互作用的NMR研究

为探讨咪唑环上取代基团对反应平衡的影响, 在模拟生理条件(0.15 mol·L-1 NaCl溶液)下, 应用多核(1H、13C和51V)、扩散排序谱(DOSY)以及变温NMR等谱学技术研究双过氧钒配合物NH4[OV(O2)2{2-(2’-Pyri-dine)-Imidazole}]·4H2O(简写为bpV(Imi-Py))和咪唑类配体(咪唑、2-甲基鄄咪唑、4-甲基-咪唑和组氨酸)的相互作用, 其从强到弱的顺序为咪唑≈4-甲基-咪唑>2-甲基-咪唑>组氨酸. 研究结果表明, 咪唑环上取代基团空间位阻对反应平衡产生较大影响,同时竞争配位的结果导致新的6 配位过氧物种[OV(O2)2L]-(L 为咪唑类配体)的生成, 当配体为4-甲基-咪唑和组氨酸时, 生成的则是一对异构体.     

Itosides A – I,New Phenolic Glycosides from Itoa orientalis

Eight new benzoylated gentisyl alcohol (=2‐(hydroxymethyl)benzene‐1,4‐diol) glucosides, itosides A–H ( 1 – 8 ), together with the new pyrocatechol (=benzene‐1,2‐diol) glycoside itoside I ( 9 ) were isolated from the bark and twigs of Itoa orientalis (Flacourtiaceae). In itosides B–D ( 2 – 4 ), the gentisyl alcohol moiety was esterified by 1‐hydroxy‐6‐oxocyclohex‐2‐ene‐1‐carboxylic acid, while itosides E–H ( 5 – 8 ) contained instead an additional 2‐hydroxybenzoic acid moiety. The compounds were accompanied by the known derivatives 4‐hydroxytremulacin ( 10 ), poliothyrsoside ( 11 ), poliothyrsin ( 12 ), homaloside D ( 13 ), tremulacin, and pyrocatechol β‐D ‐glucopyranoside. The structures of the new compounds were elucidated by spectral and chemical methods.     

5-芳胺-4,7-吲唑二酮的合成

以1,4-对醌、芳肼为原料,通过Aza-Nenitzescu反应、氧化银氧化得到吲唑醌,亲核试剂(各种芳香胺)在Ce3 催化下与吲唑醌发生迈克尔加成反应,得到一系列5-芳氨基基取代的吲唑醌.化合物结构经元素分析、IR及1H NMR证实.初步的生理活性研究表明,这些化合物具有良好的抗哮喘活性.     

改性离子液体中异丁烷与丁烯的烷基化反应

向由无水三氯化铝和盐酸三乙基胺合成的离子液体中溶入不同过渡金属（铜、铁、锌等）离子，考察它们对离子液体催化异丁烷与丁烯烷基化反应性能的影响。结果表明：过渡金属离子的加入能不同程度地影响离子液体的催化性能。溶入Cu2+和Cu+后，离子液体的催化性能有显著的改善，当Cu2+的摩尔加入量为三氯化铝的5%时，烷基化油收率达到丁烯体积的178%，对C8的选择性为75%，烷基化油辛烷值（RON）为92.2，并且离子液体可以重复使用。     

优化分离与鉴定蓝斑背肛海兔口腔神经节蛋白质组

采用双向凝胶电泳技术优化分离蓝斑背肛海兔(Notarcus leachii cirrosus Stimpson, NLCS)口腔神经节(Buccal Ganglion, BG)蛋白质组, 并获得约300个蛋白质斑点. 用组合基质辅助激光解吸电离化飞行时间(MALDI-TOF)质谱技术和胶内酶解技术测定BG蛋白质组中的96个蛋白质斑点的肽指纹(Peptide mass fingerprint, PMF)图谱. 经数据库检索与比对后, 发现96种蛋白质中仅有4种蛋白质可获得较高的匹配率, 它们分别是微管蛋白(Tubulin)、 肌动蛋白(Actin)和两个1,5-二磷酸核酮糖-羧化酶/加氧酶(Ribulose-1,5-bisphosphate carboxylase/oxygenase, Ribulose), 均属于神经细胞骨架蛋白质; 同时还发现一种交配信号肽前体(Peptide mating pheromone precursor). 利用LOCtrees软件和分类法对56种蛋白质进行亚细胞定位与分类.     

高分子路易斯酸催化剂—阳离子交换树脂四氯化锡复合物

大孔强酸性聚苯乙烯系阳离子交换树脂与SnCl_4在CS_2中反应可生成一种稳定的高分子路易斯酸催化剂.其制备简单、易分离.这种催化剂不怕水,对酯化、缩醛、缩酮、醚化及付氏烷基化反应具有较好的催化作用,且催化性能稳定,至少可重复使用10次.