水介质中Sm/BiCl~3体系促进下高烯丙基胺的合成

在THF-H~2O(4/1)介质中,Sm/BiCl~3体系促进烯丙基溴与1-(α-胺烷基)-苯并三氮唑反应,生成高烯丙基胺。反应条件中性温和,水介质操作方便,提供了合成高烯丙基胺的一条新的途径。     

人体痰液中钙的分光光度法测定

研究了钙－二甲酚橙－溴化十六烷基三甲胺－乙醇体系,并用于测定慢性肺炎患者所排痰液中的微量钙,测定结果表明,其中含钙量较人体血清中的平均钙含量高,亦高于人体细胞外液中的含量。     

高立体选择性地合成薄荷基溴和新薄荷基溴

薄荷基溴和新薄荷基溴是一类非常有用的不对称合成中间体。以L-薄荷醇为原料,通过与不同的溴化剂反应高立体选择性地得到薄荷基溴和和新薄荷基溴。当L-薄荷醇与盐酸和无水溴化锌反应时高立体选择性地得到薄荷基溴,当L-薄荷醇与三溴化磷反应时高立体选择性地得到新薄荷基溴.     

原子转移自由基聚合方法在纤维素及其衍生物改性方面的应用Ⅱ

原子转移自由基聚合反应(atom transfer radical polymerization,ATRP)是纤维素及其衍生物进行修饰改性的一种有效途径。通过ATRP对纤维素及其衍生物进行改性,可以得到不包含相应均聚物的纯接枝产物,且接枝链的长度及分子量分布均可控。通过ATRP不仅可对纤维素进行本体改性,还可对其进行表面改性。原子转移自由基聚合方法在纤维素及其衍生物改性方面的应用Ⅰ″一文介绍了通过ATRP对纤维素及其衍生物进行本体改性的研究进展。本文概述了通过ATRP对纤维素及其衍生物进行表面改性的研究进展。     

Mucoadhesive Sustained Drug Delivery System Based on Cationic Polymer and Anionic Cyclodextrin/Triclosan Complex

In this study the interactions between a cationic polymer and an anionic cyclodextrin were investigated. The system has the potential for use in a sustained release dosage forms for use on mucous membranes. As mucous membranes are negatively charged the objective of this study was to investigate whether a drug delivery system based on a cationic polymer and an anionic cyclodextrin would be more mucoadhesive than a system containing a cationic polymer and a neutral cyclodextrin. For this purpose the cationic polymer hexadimethrine bromide (HDMBr) and anionic sulfobutylether -cyclodextrin (SBECD) were utilized as well as the neutral hydroxypropyl-cyclodextrin (HPCD). Triclosan was used as a model drug. The drug delivery system was formulated as a solution or semi-solid and its adhesion to porcine buccal mucosa and cation exchange media was measured. In addition the release of triclosan from the system was quantified. No difference was observed between the two systems when they were applied to the mucosal surface. However, the formulations showed improved adhesion, compared to the neutral cyclodextrin/drug delivery system, when they could also reach the underlying surface of the excised tissue. The drug delivery system was much better retained on the cation exchange media than the uncharged system. Significant interactions were observed between the negatively charged cyclodextrin and the positively charged polymer. The results indicate that the interactions could be used to obtain a mucoadhesive sustained drug delivery system under certain circumstances. The positive charge of HDMBr did not have the expected effect on the buccal mucosa and it can be concluded that although a positive charge is likely to promote mucoadhesion, other attributes of polymers, such as molecular weight and viscosity, may have equally beneficial effect.     

正电荷聚合物动态涂敷毛细管电泳柱对碱性蛋白的分离

以１，５－二甲基－二杂氮十一烷亚甲基聚Ｎ－甲溴化物（ＨＤＢ）为添加剂对毛细管柱进行动态修饰，对４种碱性蛋白质进行分离。实验结果表明：ＨＤＢ可使电渗流（ＥＯＦ）反转，很好地抑制了碱性蛋白质在石英毛细管壁上的吸附。ＨＤＢ浓度（Ｗ／Ｖ）为０．０１２％，ｐＨ４．０～８．０之间时平均柱效为１．０ ×１０~５～１．５×１０~５理论塔板数／ｍ。每次运行之间（ｎ＝６），天与天之间（ｎ＝６），迁移时间的相对标准偏差（ＲＳＤ）分别小于１％和４％，表明该动态涂敷方法具有良好的重现性和稳定性。     

Determination of Ca, K, Mg, Na, sulfate, phosphate, formate, acetate, propionate, and glycerol in biodiesel by capillary electrophoresis with capacitively coupled contactless conductivity detection

In this work, a new method employing capillary electrophoresis (CE) for the determination of several species in biodiesel is introduced. The concentrations of inorganic species (Na⁺, K⁺, Ca²⁺, Mg²⁺, SO₄²⁻, and PO₄³⁻) and glycerol are of interest to the regulatory authorities due to their ability to form undesirable compounds in engines. Additionally, other species of low molecular weight (e.g., acetate, formate, and propionate) are of interest because they contribute towards increasing the acidity. These species are formed by the degradation of biodiesel and cause damage to engines and the environment. The cation separation was performed in background electrolyte (BGE) composed of 30 mmol L⁻¹ of 2-(n-morpholino)ethanesulfonic acid (MES)/L-histidine (His), pH 6. The separation of anionic species was carried out in similar BGE with 0.2 mmol L⁻¹ cetyltrimethylammonium bromide (CTAB) added. For glycerol, a neutral species, its oxidation with periodate was employed. This well-known reaction is specific to polyols and generates iodate. The amount of iodate produced by the reaction was determined by CE. The separation was carried out in approximately 1 min using BGE composed of 30 mmol L⁻¹ acetic acid, pH 3. The analytical parameters evaluated were: linearity (r > 0.99), the RSD values for area and migration time were < 3.4% and 0.9%, respectively, and recovery was in the range of 89 to 107%.     

Boron(III) Tribromide or Titanium(IV) Bromide and Lewis Base Promoted Baylis-Hillman Reaction

ＩｎｔｒｏｄｕｃｔｉｏｎＲｅｃｅｎｔｌｙ ,ｔｈｅＢａｙｌｉｓ Ｈｉｌｌｍａｎｒｅａｃｔｉｏｎｈａｓｂｅｃｏｍｅａｖｅｒｙｈｏｔｆｉｅｌｄｆｏｒｓｙｎｔｈｅｔｉｃｃｈｅｍｉｓｔｓ ,1 12 ｗｉｔｈａｒｅｃｅｎｔｅｘａｍｐｌｅｏｆａｃａｔａｌｙｔｉｃａｓｙｍｍｅｔｒｉｃｖｅｒｓｉｏｎ .13 ＩｔｈａｓｂｅｅｎｄｉｓｃｌｏｓｅｄｔｈａｔｔｈｅｃｏｍｂｉｎａｔｉｏｎｏｆａＬｅｗｉｓｂａｓｅｓｕｃｈａｓｃｈａｌｃｏｇｅｎｉｄｅｓ ,ａｍｉｎｅｓ ,ｐｈｏｓｐｈｉｎｅｓｏｒｑｕａｔｅｒｎａｒｙａｍｍｏ ｎｉｕｍｈａｌｉ…     

Mechanism of the Deaquation of Aquopentaaminocobalt(III) Bromide

ＩｎｔｒｏｄｕｃｔｉｏｎＴｈｅｓｏｌｉｄ ｐｈａｓｅｄｅａｑｕａｔｉｏｎ ａｎａｔｉｏｎｒｅａｃｔｉｏｎ[Ｍ(ＮＨ3 ) 5(Ｈ2 Ｏ) ]Ｘ3 → [Ｍ(ＮＨ3 ) 5Ｘ]Ｘ2 +Ｈ2 Ｏ(Ｍ =Ｃｏ3 + ,Ｃｒ3 + ｏｒＲｕ3 + ａｎｄＸ =Ｃｌ- ,Ｂｒ- ｏｒＮＣＳ- )ｈａｓｂｅｅｎｗｉｄｅｌｙｓｔｕｄｉｅｄｓｉｎｃｅｔｈｅｎｉｎｅｔｅｅｎｓｉｘｔｉｅｓ .Ｔｈｅｔｈｅｒｍａｌａｎｄｋｉｎｅｔｉｃｐａｒａｍｅｔｅｒｓｈａｖｅｂｅｅｎｃａｌｃｕｌａｔｅｄａｎｄｔｈｅｄｉｆｆｅｒｅｎｔｍｅｃｈａｎｉｓｍｈａｓｂｅｅｎｐｒｏｐｏｓｅｄａｎｄｄ…     

双模板铅离子印迹吸附剂的制备及其应用于环境水及沉积物样品中铅的选择性吸附

利用溶胶-凝胶法制备了一种双模板介孔Pb2+印迹吸附剂(Pb-CTMAB-imp).通过平衡吸附实验,研究了Pb-CTMAB-imp的吸附性能和对Pb2+的选择识别性能.结果表明,Cd2+存在时,Pb-CTMAB-imp对Pb2+的选择系数可以达到91,远高于只用十六烷基三甲基溴化铵(CTMAB)作为模板的印迹吸附剂(...