高效液相色谱法测定蜂王浆中特有成分10—羟基—2—癸烯酸的研究

本文报道反相高效液相色谱法测定蜂王浆和蜂王浆制剂中的10－羟基－2－癸烯酸（10－HDA）的方法，用二氯甲烷从蜂王浆或蜂王浆制课题占萃取10－HDA，而后用HPLC测定，实验采用YWG－C18柱，35％乙醇水溶液为流动相，己二酸为内标，紫外检测器波长为212nm，加入法测回收率在95％以上。用此法测定了鲜蜂王浆和蜂王浆制剂中的10－HDA的含量。该法简单、快速，优于气相色谱法和薄层色谱法。     

Kinetic modeling of liquid-phase adsorption of reactive dyes on activated carbon

In this paper, adsorption equilibrium and kinetics of three reactive dyes from their single-component aqueous solutions onto activated carbon were studied in a batch reactor. Effects of the initial concentration and adsorbent particle size on adsorption rate were investigated Adsorption equilibrium data were then correlated with several well-known equilibrium isotherm models. The kinetic data were fitted using the pseudo-first-order equation, the pseudo-second-order equation, and the intraparticle diffusion model. The respective characteristic rate constants were presented. A new adsorption rate model based on the pseudo-first-order equation has been proposed to describe the experimental data over the whole adsorption process. The results show that the modified pseudo-first-order kinetic model generates the best agreement with the experimental data for the three single-component adsorption systems.     

Water／Oil Biphasic Hydroformylation of Higher Olefins over a TPPTS-Rh／SiO2 Catalyst

A novel TPPTS-Rh/SiO2 catalyst, prepared by directly modifying a heterogeneous high-surface-area Rh/SiO2 catalyst with water-soluble TPPTS ligands, could decrease the resistance of masstransfer in water/oil biphasic media for the hydroformylation of higher olefins. The catalytic performancefor hydroformylation on this biphasic TPPTS-Rh/SiO2 catalyst system was higher than those of thetraditional biphasic HRhCO(TPPTS)3 systems, owing to the chemical bonds between the highly dispersedRh metal particles and the TPPTS ligands. The catalyst system is applicable for hydroformylation ofhigher olefins such as 1-dodecene.     

高效毛细管电泳前沿分析法研究酸性药物那格列奈与人血浆白蛋白的结合

用高效毛细管电泳前沿分析法研究了酸性药物那格列奈与人血浆白蛋白的结合常数、结合位点和结合率。使用未涂层的毛细管柱 (4 0cm× 5 0 μmi.d .;有效柱长 32cm) ,磷酸盐缓冲溶液 (pH 7.4 ,离子强度0 .17)为背景溶液 ,在紫外检测波长 2 14nm、运行电压 18kV和重力进样 10 0s的条件下 ,利用那格列奈谱峰的平台高度和游离药物浓度的良好线性关系 (r>0 .999,n =6 ) ,测定了那格列奈的游离药物浓度。固定药物浓度 (2 0 0 μmol L ,2 5 0 μmol L) ,考察不同的蛋白质浓度对结合的影响 ;固定蛋白质浓度 (10 0 μmol L) ,考察不同的药物浓度对结合的影响。实验数据采用非线性拟和程序进行处理 ,得到了那格列奈的蛋白质结合参数。高效毛细管电泳前沿分析法测定的数据重现性良好 (RSD <2 .5 % ,n =3) ,在药代动力学和药效学研究方面具有简便、准确的优点。     

2-(4-氯苯基)-3-甲基丁酸的消旋

以酸酐及有机惰性溶剂作混合溶剂，少量叔胺等作催化剂，2-(4-氯苯基)-3-甲基丁酸能在比较温和的条件下基本完全消旋，收率接近90％。     

高效前沿分析的发展及在药物-蛋白结合研究中的应用

介绍了高效前沿分析方法的原理、特点、种类，综述了它在药物与蛋白结合研究中的应用及国内外研究概况；通过与高效液相色谱／前沿分析比较，阐明了毛细管电泳／前沿分析在药物蛋白结合研究中的优势；分析了在药物与蛋白结合研究中所采用的各种研究方法，通过与这些研究方法的比较，阐明了高效前沿分析的优越性及其广阔的应用前景，同时提出了在高效前沿分析方法中有待完善和注意的问题。     

The effect of annealing on the subsequent cold crystallization of amorphous poly(ethylene terephthalate)

Amorphous poly(ethylene terephthalate) was annealed at temperatures around the glass transition temperature and then heated up in differential scanning calorimeter at 20 °C min⁻¹. It was found that the annealing favored the subsequent cold crystallization and this effect became stronger with increasing annealing temperature. The experimental results were explained by considering the structural change during the annealing.     

Maleic acid-styrene encapsulated silica cation exchanger in high performance liquid chromatography

The use of poly(maleic acid–styrene)-encapsulated silica for the determination of monovalent and divalent cations is well accepted in ion chromatography. The separation of Mn²⁺, alkali and alkaline earth metal cations is obtained under the same chromatographic conditions. The influences of pH and the concentration of eluent on the retention of cations have been studied. The preparation conditions of packings were studied. The metal ions in the boiler water samples from a thermal power plant were quantitatively determined using this column. The results are in agreement with those determined by ICP and Volumetric analysis methods.     

Tetrapyrrole derivatives substituted with ferrocenylethynyl moieties. synthesis and electrochemical studies

Up to eight redox-active ferrocenyl units have been incorporated, through the unsaturated ethynyl linkers, on the periphery of a series of cyclic tetrapyrrole derivatives including zinc(II) phthalocyanine and 2,3-naphthalocyanine, and nickel(II) meso-diphenylporphyrin. The synthesis of the former two macrocycles 4 and 7 involves the Sonogashira coupling reaction of ferrocenylethyne with 4,5-dichlorophthalonitrile (1) or 6,7-dibromonaphthalonitrile (5), respectively, followed by a base-promoted cyclization. The meso-bis(ferrocenylethynyl)porphyrin 11 has been prepared from the dibromo analogue 10 also by a palladium-catalyzed coupling reaction. These novel macrocyclic compounds have been spectroscopically and electrochemically characterized. As revealed by cyclic voltammetry, the ferrocenyl moieties appear to be electrochemically independent in these complexes and there is no significant electronic coupling among the iron(II) centers.     

在线固相萃取和高效液相色谱法测定卷烟主流烟气中几种芳胺

研究了用在线固相萃取富集和高效液相色谱法测定卷烟主流烟气中的几种芳胺(苯胺、对甲基苯胺、2,4-二甲基苯胺、1-萘胺、2-萘胺和4-氨基联苯)的方法,样品中的芳胺用邻甲氧基酚衍生生成偶氮染料,偶氮染料用WatersXterraTMRP18色谱柱在线固相萃取富集,然后以WatersXterraTMRP18色谱柱为固定相,75%的甲醇(内含0.01mol/LpH=8的四氢吡咯-醋酸缓冲液)为流动相分离,二极管矩阵检测器检测;苯胺、对甲基苯胺、2,4-二甲基苯胺、4-氨基联苯、1-萘胺、2-萘胺的检出限分别为005、0.08、0.08、0.06、0.03和0.03μg/L。几种芳胺的相对标准偏差在2.2%~3.4%之间;标准回收率在89%~106%之间,方法用于卷烟主流烟气中几种芳胺的测定,结果令人满意。