A new long-side-chain sulfonated poly(2,6-dimethyl-1,4-phenylene oxide)(PPO)/polybenzimidazole(PBI)amphoteric membrane for vanadium redox flow battery

A new amphoteric membrane was prepared by blending long-side-chain sulfonated poly(2,6-dimethyl-1,4-phenylene oxide)(S-L-PPO)and polybenzimidazole(PBI)for vanadium redox flow battery(VRFB)application.An acid-base pair structure formed between the imidazole of PBI and sulfonic acid of S-L-PPO resulted in lowered swelling ratio.It favors to reduce the vanadium permeation.While,the increased sulfonic acid concentration ensured that proton conductivity was still at a high level.As a result,a better balance between the vanadium ion permeation(6.1×10^-9 cm^2·s^-1)and proton conductivity(50.8 m S·cm^-1)in the S-L-PPO/PBI-10%membrane was achieved.The VRFB performance with S-L-PPO/PBI-10%membrane exhibited an EE of 82.7%,which was higher than those of pristine S-L-PPO(81.8%)and Nafion 212(78.0%)at 120 m A·cm^-2.In addition,the S-LPPO/PBI-10%membrane had a much longer self-discharge duration time(142 h)than that of Nafion 212(23 h).

Synthesis, Crystal Structure and Property of a Series of Supramolecular Polymers Based on Novel 3,5-Dimethyl- 2,6-bis(3-(pyrid-2-yl)-1,2,4-triazolyl)pyridine Ligand

Solvothermal reactions of 3,5-dimethyl-2,6-bis（3-（pyrid-2-yl）-1,2,4-triazolyl） pyridine （L）, 1,4-benzendicarboxylic acid （H2bdc）, and transitional metal cations of M11 （M = Mn, Co, Cd） in the presence of oxalic acid （H2ox） afford three novel supramolecular polymers （CPs）, namely, {[M2（ox）（L）2][bdc][M2（Hox）2（OH）（H2O）4]·3H2O}n （M = Mn for 1, Co for 2, Cd for 3）. Single-crystal X-ray diffraction analysis reveals that complexes 1-3 are isostructural and the 3D supramolecular structure was connected through non-covalent interactions. With the help of H2ox, the L ligands cheated with center atoms forming a butterfly [M2（ox）（L）2]2＋ building block. The bdc2- ligand linked with the unprecedented [M2（Hox）2（OH）2（H2O）4] units through strong O-H...O hydrogen bonds forming a zigzag chain, which are further connected through π-π interactions between L and bdc2- ligands to form a 3D supramolecular structure. Moreover, elemental analyses, IR, thermogravimetric, PXRD and luminescence have been investigated.

Facile and Efficient Syntheses of (±)-2,6-Dimethyl-6-hydroxy-2,7-octadienoic Acid and Its Methyl Ester

The facile and efficient total syntheses of monoterpenoid acid 7a and its ester 7b, isolated from Artemisia siebert and Piper aduncum respectively, can be completed in four steps with an overall yield 41%.

雷公藤内酯酮与2,6-二甲基-β-环糊精包合物的制备及性能研究

通过饱和水溶液法制备了雷公藤内酯酮(TN)和2,6-二甲基-β-环糊精(DM-β-CD)的包合物,采用一维核磁共振氢谱(1H NMR)、二维核磁共振氢谱(2D NMR)、傅里叶变换红外光谱(FT-IR)、X射线衍射(XRD)、扫描电子显微镜(SEM)和热重分析(TG)等技术对TN/DM-β-CD包合物进行表征,推测可能的包合模式。Job曲线法表明,主客体的包合比为1∶1,采用紫外-可见光谱滴定法测定得稳定常数为2891 L/mol。形成包合物后,TN的水溶解度由0.0018 mg/mL增至2.7 mg/mL,提高了150倍。体外释放实验表明,在12 h时包合物累积释放率可达70%,而TN累积释放率达70%需120 h。本研究为制备较高水溶性和低毒性的天然药物活性分子提供了新途径。

2,6-二甲基-3-乙基-β环糊精的合成

以 β 环糊精为原料 ,经烷基化分两步取代羟基 ,合成了 2 ,6 二甲基 3 乙基 β环糊精 ,并用IR与H1 NMR将两步合成产物作了定性描述 。

卟硒啉-2,6-二甲基-β-环糊精包合物的表征及注射液的制备

本文通过饱和水溶液法制备卟硒啉-2,6-二甲基-β-环糊精包合物,以提高卟硒啉的溶解度,从而得到其注射液。通过高效液相色谱(high performance liquid chromatography,HPLC)法对包合物中的卟硒啉含量进行检测,再以包合率为指标,正交设计优化制备工艺。采用X射线衍射(X-ray diffraction,XRD)、傅里叶变换红外光谱(Fourier-transform infrared spectroscopy,FTIR)、扫描电子显微镜(scanning electron microscope,SEM)对包合物结构进行验证,同时考察包合物对卟硒啉溶解度及其稳定性的影响。结果显示,优化的制备工艺条件质量比为1∶340、包合时间为3 h、包合温度为70℃,制得的包合物的包合率为(91.24±0.42)%,XRD、FTIR、SEM结果均证明了包合物形成。卟硒啉-2,6-二甲基-β-环糊精包合技术能显著提高卟硒啉溶解度且所建立的HPLC法对卟硒啉含量的检测快速简便、准确、适用性强、专属性高、重复性好,可用于卟硒啉环糊精包合物中的卟硒啉的含量检测,为卟硒啉新剂型的开发及临床应用奠定基础和提供技术支持。

七-(2,6-二甲基)-β-环糊精对木犀草素的增溶研究

目的研究5种环糊精对木犀草素(luteolin,Lut)的增溶作用,探讨了环糊精对难溶性药物的增溶机理。方法采用相溶解度法比较了β-环糊精(β-cyclodextrin,β-CD)、γ-环糊精、2-羟丙基-β-环糊精、七-(2,6-二甲基)-β-环糊精[heptakis-(2,6-dimethyl)-β-cyclodextrin,DM-β-CD]与6-葡萄糖基-β-环糊精对Lut的增溶作用,采用傅里叶变换红外光谱法(Fourier transform infrared spectroscopy,FT-IR)、X射线粉末衍射法(X-ray diffraction,XRD)等手段表征了DM-β-CD与Lut形成的复合物,采用分子对接与分子动力学推测了复合物结构。结果5种环糊精中DM-β-CD具有对Lut的最佳增溶作用,在浓度为2.5×10^−3 mol·L^−1时,Lut溶解度为1.56×10^−4 mol·L^−1,是纯水中溶解度的6.37倍;FT-IR与XRD表征了DM-β-CD/Lut复合物结构,主客体之存在弱相互作用;分子对接结果显示在复合物中,Lut的中A环与C环复合在DM-β-CD空腔中,B环位于DM-β-CD的大口处,主客体之间存在多个氢键作用;分子动力学模拟显示DM-β-CD/Lut复合物在5 ns内结构稳定,未发生较大形变,主、客体均方根差分别为2.6320与0.4754Å。结论DM-β-CD可有效提高Lut溶解度,增溶作用机理是二者之间形成了复合物。

Synthesis of Folate-Appended <i>β</i>-Cyclodextrin Using Phenanthroline as Linker for Cancer Targeting Drug Delivery

Here we have synthesized cancer targeting drug delivery system that contains β-cyclodextrin as a drug carrier and folic acid as a targeting ligand. Folic acid was selected as a cancer targeting ligand because folic acid receptors are highly expressed in a variety of tumor types. β-cyclodextrin and folic acid were connected through a linker [1,10-phenanthroline or 5-(hydroxymethyl) furfural]. β-cyclodextrin and folic acid were attached to the linker by formation of Schiffbase and ester, respectively. Our targeted synthetic products were confirmed by NMR, Mass and IR spectroscopy. We anticipate that our synthetic products can confer cancer cell-specific drug delivery as well as desired properties such as nanoparticle formation.

冷水七的化学成分研究

通过正丁醇萃取、硅胶柱色谱、Sephadex LH-20以及HPLC等色谱手段对凤仙花科凤仙花属植物冷水七的50%乙醇提取物进行分离纯化,并结合1D-NMR,2D-NMR,HRESI-MS等数据进行结构鉴定。共分离鉴定8个化合物,1为新化合物,命名为2,6-dimethyl-2-vinyl-2,3,4,7-tetrahydrooxepine(1),其余7个为已知化合物,分别是1,3,6-trihydroxy-7-methyl-anthraquinone(2),4-hydroxybenzaldehyde(3),4-(3-methoxy-4-hydroxyphenyl)-2-butanone(4),podophyllotoxin(5),scopoletin(6),α-spinasterol(7)和3-O-β-D-glucopyranosyl-α-spinasterol(8)。以上已知化合物均为首次从该植物中分离得到。