液相色谱手性拆分机理的热力学方法研究

手性识别是分子识别的一个重要组成部分。液相色谱手性拆分机理研究有助于色谱条件的优化和新型手性固定相的设计,也有助于理解手性识别机制。本文就线性色谱与非线性色谱条件下手性拆分过程对应热力学参数的推求方法进行了评述,阐述了相关热力学参数的涵义及其在色谱保留及手性拆分机理探讨中的应用,并展望了该领域的研究前景。     

苯乙烯/马来酸酐共聚物修饰碳纳米管的研究

利用羟基碳纳米管上的羟基与马来酸酐之间的简单反应, 在碳纳米管上引入双键, 进一步引发苯乙烯聚合, 在碳纳米管表面接枝苯乙烯马来酸酐共聚物, 同时采用羟基碳纳米管与苯乙烯马来酸酐共聚物直接反应也在碳纳米管的表面引入了苯乙烯马来酸酐共聚物. 经IR, Raman, TG和TEM测定, 证明了碳纳米管与苯乙烯马来酸酐共聚物之间为化学键连接关系.     

A Novel High Active TiO2/AC Composite Photocatalyst Prepared by Acid Catalyzed Hydrothermal Method

A high active novel TiO2/AC composite photocatalyst was prepared and used for phenol degradation. It was much more active than P-25 and exhibiting good decantability, less deactivation after several runs and less sensitive to pH change. Diffuse reflectance spectra (DRS) revealed that the electronic change in TiO2 did not occur by the addition of AC. Results of SEM and XRD suggested that better TiO2 distribution can be achieved when optimal AC content was adopted. The performance of the prepared TiO2/5AC catalyst revealed great practical potential in wastewater treatment field.     

高效液相色谱/电化学法测定大鼠血液和脑组织中单胺类物质的含量

建立了高效液相色谱／电化学检测法测定大鼠脑组织和血液中单胺递质及其代谢产物的方法。能同时测定去甲肾上腺素（NE）、肾上腺素（E）、3,4-二羟基苯乙酸（DOPAC）、多巴胺（DA）、高香草酸（HAV）、5-羟色胺（5-HT）,并能和内标3,4-二羟卞胺（DHBA）分离良好。本方法快速、简便,回收率为92％-105％,线性范围2．8-680ng／mL,检出限为0．05ng（S／N=3）。本方法已应用在服用中药的大鼠下丘脑组织及血液的测定中,数据显示,本法能满足测定要求。     

配位作用毛细管电泳方法研究

研究了一种以过渡金属离子为添加剂,基于配位相互作用的毛细管电泳技术。选择7种芳香胺类化合物作为分析对象,考察了金属离子种类和浓度、运行介质酸度、电压对配位毛细管电泳的影响。通过对邻苯二胺变质样品的鉴别以及实际合成药磺胺类药物的分离,考察了这种毛细管电泳分离技术的分离能力,效果令人满意。应用于颠茄磺苄啶片中磺胺甲噁唑(SMZ)的定量测定时,SMZ的检出限为0.12 mmol/L;线性范围为0.25~10 mmol/L(r2=0.9917);平均加样回收率为97.8%,表明所建立的配位作用毛细管电泳(C ICE)方法,具有稳定、可靠的定性和定量分析能力。     

A NOVEL ZWITTERIONIC SILANE COUPLING AGENT FOR NONTHROMBOGENIC BIOMATERIALS

A novel silane coupling agent bearing sulfobetaine group, N,N-diethyl-N-（3-sulfopropyl）-aminopropyl- trimethoxysilane （DESATS）, was first designed, synthesized and characterized. Its solution property was studied by means of dynamic light scattering. DESATS was successfully bonded onto the surface of the glass and proved by ESCA. Platelet adhesion assay in vitro indicated that the nonthrombogenicity of glass slide modified with DESATS is greatly improved.     

两个含有平行交替链的新型二氰胺配位高聚物: {Mn(dmpz)[N(CN)2]2}2和{Cu(dmpz)[N(CN)2]2}2

Two new dicyanamide coordination polymers, {Mn(dmpz)[N(CN)2]2}2 (1) and {Cu(dmpz)[N(CN)2]2}2 (2)(dmpz=3,5-dimethylpyrazole), were synthesized and characterized by single crystal X-ray diffraction analysis and IR spectroscopy. In 1 and 2 the metal ions have two different coordination modes, where one is coordinated to four dicyanamide anions and two monodentate dmpz molecules to form a slightly distorted octahedral geometry, while the other adopts octahedral geometry, surrounded by four nitrile N atoms and two amide N atoms of the dicyanamide anions. Both complexes contain two alternating chains that are parallel to each other.     

Development and validation of a liquid chromatography/tandem mass spectrometry procedure for the quantification of adefovir in human plasma

To investigate the pharmacokinetics of adefovir as an anti-hepatitis B virus drug, a sensitive and specific liquid chromatography/tandem mass spectrometry method was developed and validated. After a simple protein precipitation using methanol, the post-treatment samples were analyzed on a C(18) column interfaced with a triple-quadrupole tandem mass spectrometer using positive electrospray ionization. A structural analogue, PMPA, was used as the internal standard. The method was linear in the concentration range 0.25-100 ng/mL. The lower limit of quantification was 0.25 ng/mL. The intra- and inter-day relative standard deviation over the entire concentration range was 5.7% or less. The accuracy determined at three concentrations (0.75, 10 and 80 ng/mL for adefovir) was within +/-2.5% relative error. The method described here was successfully applied for the evaluation of pharmacokinetic profiles of adefovir after single oral administration doses of 5, 10 and 20 mg adefovir dipivoxil to ten healthy volunteers.     

EPR studies on H-abstractions/spin-trapping reactions of new 'magic blue' reagents with alcohols

The H-abstractions/spin-trapping reactions with primary, secondary and tertiary alcohols of new 'magic blue' reagents, namely, the blue F113 (CClF₂CCl₂F) solution containing bis{perfluoro[1-(2-fluorosulfonyl)ethoxy]ethyl} nitroxide (2) and perfluoro[1-nitroso-1-(2-fluorosulfonyl)ethoxy]ethane (3) both generated in the reaction of perfluoro[2-(2-fluorosulfonyl)ethoxy]propionyl peroxide (1) with sodium nitrite in F113 at room temperature, were studied by EPR. Based on the interpretation of the EPR spectra of the spin adducts, nitroxides, the region-selectivity of H-abstraction has been disclosed and the possible mechanistic paths of H-abstraction have also been discussed. EPR of H-abstraction by using 'magic blue' reagents can also be used for producing various hydroxyalkyl radicals from common alcohols.     

海藻多糖的组成及结构光谱分析

海藻多糖具有抗凝血等多种生物活性,其活性与多糖的组成结构有关。本文对近年来红藻、褐藻及少量绿藻多糖的单糖组成及含量研究以及FT-IR和12^C NMR两种主要光谱手段对多糖结构研究的结果进行了介绍。