The influence of 1-butyl-3-methyl-imidazolium bromide on the partitioning of l-tyrosine within the {polyethylene glycol 600 + potassium citrate} aqueous biphasic system at T = 298.15 K

Partitioning in aqueous biphasic systems (ABS) is widely recognized today as a rapid, gentle, and highly efficient technique for the separation of soluble as well as particulate biomaterials. This technique has gained increasing attention as the separation method of choice in biotechnology. In recent years, a new approach has been proposed based on the use of ionic liquids (ILs) as adjuvants for the separation and purification of bio-molecules using polymer-based ABS. In this regard, the influence of IL 1-butyl-3-methylimidazolium bromide ([C₄mim]Br) on the phase behavior and extraction capability of {PEG 600 + tri-potassium citrate (K₃C₆H₅O₇)} ABS for l-tyrosine (Tyr) is investigated here. For this purpose, phase diagrams and the liquid–liquid equilibrium (LLE) data for the {PEG 600 + K₃C₆H₅O₇} ABS with the addition of small quantities of IL were determined at T = 298.15 K. It was found that, for the studied polymer-based ABS, the addition of 5 wt% of [C₄mim]Br to ABS caused the expansion of two-phase area in the salt-rich region; while, for the PEG-rich region no change was observed. The partition coefficients of l-tyrosine (K_Tyr) within the studied system were determined at T = 298.15 K. The results obtained indicate that the addition of small quantities of [C₄mim]Br to the {PEG 600 + K₃C₆H₅O₇} ABS could enhance the extraction efficiency for l-tyrosine. In addition, the experimental data are correlated using the NRTL model. The comparisons between the correlation and the experimental data reveal a good agreement.     

Determination of Metal Ions by High Performance Liquid Chromatography

The mixture of metal ions [Bi(III), Fe(III), Fe(II), Cu(II), Zn(II), Ni(II), Co(II), Pb(II), Cd(II), Mn(II)] were separated in the bonded-phase strong cation exchange column (Vydac-401 SA) and monitored at 540 nm after a postcolumn reaction with 4-(2-pyridylazo)-resorcinol (PAR). Citrate, tartrate, lactate and α-hydroxyisobutyrate buffer were used as eluent and it has been found that the elution order of some metal ions were changed with different eluents. The detection limits and the calibration curves of metal ions were also studied.     

Aqueous Synthesis of Water-Soluble Citrate-Modified Cadmium Selenide/Cadmium Sulfide/Zinc Sulfide Quantum Dots

Water-soluble cadmium selenide/cadmium sulfide/zinc sulfide core/shell/shell quantum dots were synthesized in aqueous solution using trisodium citrate as modifier. The crystal structure, morphology, component, and spectral properties of cadmium selenide/cadmium sulfide/zinc sulfide core/shell/shell quantum dots were characterized by X-ray power diffraction, transmission electron microscope, energy dispersive X-ray analysis, infrared spectrum, ultraviolet–visible absorption spectrum, and fluorescence spectrum. The results show that the spherical citrate-modified cadmium selenide/cadmium sulfide/zinc sulfide core/shell/shell quantum dots with diameter around 3.6 nm belong to the cubic zinc blende structure. The citrate-modified cadmium selenide/cadmium sulfide/zinc sulfide core/shell/shell quantum dots show a narrow, symmetric, and strong fluorescence emission spectrum band with narrow full width at half maximum of 53 nm, and the fluorescence quantum yield can reach up to 37.3%. The high-quality citrate-modified cadmium selenide/cadmium sulfide/zinc sulfide core/shell/shell quantum dots with good fluorescence properties have potential for application in biological fluorescence analysis.     

一步可控合成二氧化硅纳米管和空心球

通过简单的溶胶凝胶法在相同体系中可控合成了新颖有序的二氧化硅纳米管和空心球,对制备二氧化硅纳米管的多种反应条件进行了系统研究。发现反应时间、溶液中水和乙醇比例、搅拌和滴加速度对形成管状结构都有着重要影响。同时,纳米管的形成机理研究表明,在醇水混合溶液中柠檬酸三铵晶体为细柱状形貌,其作为重要的结构导向剂为二氧化硅胶晶附着提供模板,从而形成管状结构,二氧化硅空心球也显示了相似的形成过程。     

Preparation of heterogeneous catalysts

The preparation of heterogeneous catalysts has been for many years a dynamic field of sub-nanotechnology and remains so nowadays. The approach to preparation must be examined in function of the specific demands concerning (i) activity and (ii) selectivity, that both depend on the arrangement of atoms at a scale smaller than 0.02 nm. Adequate access of reactants to the surface must be provided. Most catalysts are used in the form of pellets or cylinders obtained by pressing, extrusion or other techniques. This implies a control of texture at dimension scales extending from a fraction of a nanometer to several millimetres (and sometimes more). A third demand (iii) is resistance to ageing. In particular, stability at relatively high temperatures is necessary.The strategy adopted in the majority of cases is to start from a material that is homogeneous in composition at the Angström scale, generally a liquid or a solid of complex composition, frequently amorphous. A general objective is to locate the different constituting atoms at precise positions. The main difficulty is to transform the starting precursor into a highly porous solid without segregation of different elements that would produce tiny parts with different properties.The specific approach to catalyst preparation is based on the general concepts used for controlling the reactivity of solids. Typical methods of general use will be examined. Chemical bonds of practically any kind can retain the elements constituting the future catalyst at the position they have in the precursor. The so-called ‘citrate process’ and its variants are of wide application. More elaborate approaches start from molecules or polymers associating the necessary elements.     

光度法测定枸橼酸西地那非及尿中西地那非的含量

枸橼酸西地那非(Sildenafil citrate)商品名为万艾可(Viagra),是治疗男性性功能障碍药。目前测定西地那非含量的方法主要是HPLC,操作繁琐,仪器昂贵。本文在pH2．5-4．7的酸性介质中,发现乙基曙红(EE)与西地那非(SD)反应后,生成红色离子缔合物,其最大显色波长和最大褪色波长分别为550nm和520nm,表观摩尔吸光     

过氧草酸酯-四溴荧光素化学发光法测定多巴胺

对过氧化草酸酯化学发光体系的不同催化剂及荧光试剂进行了研究和比较,基于化学发光的强度和时间曲线,提出了以柠檬酸钠为催化剂和四溴荧光素为荧光试剂的化学发光反应新体系,用于有多巴胺反应生成的过氧化氢的测定.多巴胺线性方程Iα =22.95+0.21c,检出限为1.40 nmol/L,线性为2～1 000 nmol/L,灵敏度高、干扰少,用于针剂中多巴胺测定,回收率94.5％(n=11),结果令人满意.     

正丁烷在金属钼酸盐催化剂上的氧化脱氢

 用柠檬酸盐法合成了第一系列过渡金属(Cr,Mn,Fe,Co,Ni,Cu和Zn)及Mg的钼酸盐催化剂,研究 了它们对正丁烷氧化脱氢反应的催化作用. 结果表明,这些钼酸盐催化剂的催化性能受阳离子的影响较大. CoMoO4催化剂具有最高的催化活性和较高的选择性,其催化性能与文献报道的对正丁烷氧化脱氢反应催化性能最好的ZrP2O7和Mg3V2O8催化剂大致相当; MgMoO4催化剂虽然选择性较高,但活性较低; Cr2(MoO4)3上基本没有C4烯烃生成; 其它钼酸盐催化剂对正丁烷氧化脱氢反应的催化活性和对烯烃的选择性都较低. XRD,NH3-TPD和H2-TPR的研究结果表明,催化剂为单一的钼酸盐晶相,催化剂的性能由其氧化还原性决定而与其表面酸量没有直接关系. 通过对产物分布的分析,提出了正丁烷在CoMoO4催化剂上的氧化脱氢反应途径. 在558 ℃,正丁烷发生氧化脱氢生成正丁烯和丁二烯以及氧化燃烧生成CO2三个平行竞争反应的竞争分率分别约为75%,10%和15%. 在正丁烷转化率较高的条件下,产物中的CO2主要来自C4烯烃的再氧化反应,而CO则完全来自C4烯烃的再氧化.     

药用甜菜碱柠檬酸盐的合成研究及中试

目的研究医药级甜菜碱柠檬酸盐适合工业化生产的合成工艺。方法由氯乙酸三甲胺和柠檬酸合成甜菜碱柠檬酸盐,并对合成条件进行了讨论和中试实验放大,对产物进行了表征及含量测定。结果产物结构由IR和元素分析得到证明,产物含量用非水滴定法进行了测定。最佳工艺条件下收率92.03%,纯度99.1%,并在设计的中试装置中进行了放大实验,工艺放大效应不明显。结论合成工艺及放大实验表明,工艺适用于工业规模制备医药级甜菜碱柠檬酸盐。     

柠檬酸钠对L–缬氨酸发酵及代谢流量分布的影响

以黄色短杆菌XV0505为供试菌,研究柠檬酸钠对L–缬氨酸发酵的影响,同时应用MATLAB软件和代谢流量分析方法,定量研究柠檬酸钠对L–缬氨酸发酵中后期胞内代谢流量分布的影响.结果表明,添加2.0 g/L柠檬酸钠可提高L–缬氨酸产量,同时不影响菌体生长.添加柠檬酸钠后,L–缬氨酸生物合成的代谢流从41.42增长至45.87,较未添加前提高了10.74%.合成副产物L–丙氨酸和HAc的代谢流明显减少,分别降低了21.10%和32.47%.因此,添加柠檬酸钠能够扰动L–缬氨酸生物合成途径关键节点代谢流量分布,有利于减少副产物的生成,提高L–缬氨酸生物合成途径的代谢流量.