纳米复合光催化剂TiO2-ZrO2的制备、表征及其光催化活性

通过溶胶-凝胶技术制备了不同比例(3:1、1:1、1:3)的纳米复合光催化材料TiO2-ZrO2,采用XRD、N2吸附、SEM-EDX和TPD等测试手段对其进行了表征,探讨了比例不同的TiO2-ZrO2结构的变化规律以及这种变化对催化剂催化活性的影响.通过紫外区和可见区的光催化降解染料亚甲基蓝、罗丹明B的实验,考察了其光催化活性.实验结果表明,不同比例的纳米复合光催化材料TiO2-ZrO2的催化活性均高于单体TiO2和单体ZrO2.     

水溶性β-CD聚合物在毛细管电泳中分离氨基酸对映体

以环氧氯丙烷（EP）为交联剂,合成水溶性的β-环糊精聚合物（β-CDpoly-met）,提出了一种以β-CDpolymer为手性选择剂,在毛细管电泳中分离未衍生芳环氨基酸对映体的方法。考察了手性选择剂浓度、背景电解质溶液pH、柱温及分离电压对分离的影响。在优化的实验条件下,使3种氨基酸对映体得到了基线分离。     

顶空液相微萃取-气相色谱法测定盐酸雷尼替丁中二氯甲烷和三氯甲烷的残留量

采用顶空液相微萃取与气相色谱联用技术测定雷尼替丁中二氯甲烷和三氯甲烷的残留量。自制了萃取液保护装置。考察了萃取溶剂的种类、萃取时间、萃取温度、萃取液的体积对二氯甲烷和三氯甲烷萃取效果的影响。以正十三烷为萃取剂,在60 ℃下萃取30 min,萃取液滴体积2 μL。二氯甲烷含量在1～10 μg/g范围内与色谱峰高呈线性关系,相关系数(r2)为0.9733;三氯甲烷含量在1～10 μg/g范围内与色谱峰高呈线性关系,r2为0.9724。二氯甲烷和三氯甲烷的最低检出限分别为0.0273 μg/g和0.0410 μg/g,加标回收率分别为93.6%～102%和98.1%～103%。方法简便易行,测定结果准确。     

有序介孔材料H6P2W18O62/TiO2(Brij-76)的制备与微波增强光催化降解一氯苯

采用非离子表面活性剂C18H37(OCH2CH2)10OH(Brij-76)作为模板剂, 在以杂多酸H6P2W18O62对TiO2掺杂改性基础上, 通过模板-溶胶-凝胶-程序升温溶剂热一步法在较低温度下制备了有序复合介孔材料H6P2W18O62/TiO2(Brij-76). 通过傅立叶变换红外(FT-IR)光谱, X射线衍射(XRD), 扫描电子显微镜(SEM), 能量色散X射线(EDX), N2吸附-脱附测定和NH3程序升温脱附(NH3-TPD)等手段对其进行了表征. 结果表明, 以非离子表面活性剂Brij-76为模板剂制得的复合材料H6P2W18O62/TiO2(Brij-76)平均孔径约为3.31 nm, BET比表面积为99.78 m2·g-1. 与TiO2相比, 其孔径有序性大幅度提高, 粒子的聚集度降低, 表面酸性显著增加. 微波增强光催化性能研究结果显示, H6P2W18O62/TiO2(Brij-76)在微波作用下催化活性更高, 可有效地降解一氯苯溶液.     

Theoretical prediction regarding structural and thermodynamical characteristics of stable CH3PO2 isomers and unimolecular decomposition mechanisms of species CH3P(O)2, CH3O?PO,and CH2P(O)OH

The detailed isomerization and dissociation reaction potential energy profile of the CH₃PO₂ system was established at the UCCSD(T)/6‐311++G(3df,2p)//UB3LYP/6‐311++G(d,p) level of theory. Seventy minimum isomers were located and connected by 93 optimized interconversion transition states. Furthermore, 32 isomers with high kinetic stability were predicted to be possible candidates for further experimental detection. The bonding nature of the suggested stable isomers was analyzed while their molecular properties including heats of formation, adiabatic ionization potentials, and adiabatic electronic affinities were calculated at the G2, G2(MP2), G3, and CBS‐Q levels. Based on the isomerization and dissociation potential energy surface, possible unimolecular decomposition mechanisms and pathways of the low‐lying molecules CH₃P(?O)₂, CH₃O? P?O, and CH₂?P(?O)OH were discussed. Furthermore, the transition state theory rate constants of the primary unimolecular dissociation channels were also calculated. © 2009 Wiley Periodicals, Inc. J Comput Chem, 2009     

烯丙基-β-环糊精基手性毛细管电色谱整体柱的一步法制备及其性能

以烯丙基-β-环糊精、甲基丙烯酸缩水甘油酯和乙二醇二甲基丙烯酸酯为功能单体,一步键合制备了环糊精聚合物毛细管整体柱.在电色谱模式下18种氨基酸对映体得到成功分离.研究发现,将修饰的环糊精衍生物作为功能单体制备出的毛细管整体柱对疏水性,含氨基和苯环的手性化合物具有良好的保留行为,并具有良好的稳定性和重现性.新型电色谱柱也被应用于手性药物的分离.     

甲基丙基酸丁酯/SiO2/TiO2有机-无机杂化毛细管整体柱的制备及应用

采用溶胶-凝胶法制备了SiO2/TiO2杂化材料,并通过双官能团试剂3-(甲氧基硅烷基)甲基丙烯酸丙酯(γ-MAPS)对其进行改性;改性溶胶与甲基丙基酸丁酯(BMA)作为功能单体,在毛细管中进行原位聚合反应,制备了新型的有机-无机杂化毛细管整体柱。 采用扫描电子显微镜观察了整体柱柱床的形貌。 以硫脲为电渗流标记物对所制备的整体柱进行了柱性能评价,考察了柱的稳定性和重现性,获得了88000 plates/m的柱效;考察了中性物质在柱上的的保留行为,得出该柱具有反相电色谱保留性能。 通过对2种短肽(磷酸肽和非磷酸肽)洗脱测试,实现了对磷酸肽的有效富集与分离。     

Competitive Assay for Theophylline Based on an Abasic Site‐Containing DNA Duplex Aptamer and a Fluorescent Ligand

A fluorescence assay for theophylline, one of the common drugs for acute and chronic asthmatic conditions, has been developed based on an abasic site‐containing DNA duplex aptamer (AP aptamer) in combination with an abasic site‐binding fluorescent ligand, riboflavin. The assay is based on the competitive binding of theophylline and riboflavin at the abasic (AP) site of the AP aptamer. In the absence of theophylline, riboflavin binds to the receptor nucleotide opposite the AP site, which leads to fluorescence quenching of the riboflavin. Upon addition of theophylline, competitive binding occurs between theophylline and riboflavin, which results in an effective fluorescence restoration due to release of riboflavin from the AP site. From an examination of the optimization of the AP aptamers, the complex of riboflavin with a 23‐mer AP aptamer (5′‐TCT GCG TCC AGX GCA ACG CAC AC‐3′/5′‐GTG TGC GTT GCC CTG GAC GCA GA‐3′; X : the AP site (Spacer C3, a propylene residue)) possessing cytosine as a receptor nucleotide was found to show a selective and effective fluorescence response to theophylline; the limit of detection for theophylline was 1.1 μM . Furthermore, fluorescence detection of theophylline was successfully demonstrated with high selectivity in serum samples by using the optimized AP aptamer and riboflavin.     

高效液相色谱-手性流动相添加法拆分盐酸丙胺卡因对映体

以羧甲基-β-环糊精(CM-β-CD)为手性流动相添加剂,提出了拆分盐酸丙胺卡因对映体的高效液相色谱法。选用C18色谱柱,流动相为含0.4g·L-1的CM-β-CD的甲醇-乙腈-水(60+15+25)溶液,紫外检测波长为202nm,进样量为10μL,流量为0.4mL·min-1。结果表明:盐酸丙胺卡因对映体得到良好的分离,分离度为1.41。     

含水溶液中香豆素类探针对碘离子的荧光增强识别

设计合成了新型含硫代半卡巴肼结构的香豆素类I-荧光分子探针CI,其结构用1H NMR,13C NMR,GC/MS和元素分析进行了表征,并考察了其光谱性能.结果表明CI在中性缓冲溶液中,在常见阴离子(F-,Cl-,Br-,I-,AcO-,HSO-4,H2PO-4)中能够专一性地识别I-.滴加I-后引起吸收光谱蓝移80 nm,荧光光谱蓝移6 nm,荧光增强5.9倍,溶液荧光由黄绿色变为亮蓝色.其它阴离子的存在并未干扰CI对I-的检测.