超高效液相色谱-串联质谱法测定蜂蜜中胆碱和乙酰胆碱

建立了超高效液相色谱-串联质谱同时测定蜂蜜中胆碱和乙酰胆碱的分析方法.试样采用水-乙腈(体积比2:3)溶液提取,乙腈-水(体积比8:2)稀释后以0.22μm滤膜过滤上机测定.采用ACQUITY UPLC BEH HILIC(100 mm×2.1 mm,1.7μm)色谱柱分离,以10 mmol/L乙酸铵(含0.1％乙酸)...     

铜掺杂钙铝水滑石催化氧化异丙苯制备异丙苯过氧化氢

采用共沉淀法制备了铜掺杂钙铝水滑石Ca₄Cu _x Al-LDHs（x=0,0.1,0.3,0.5,0.8,1.0）,并对其催化异丙苯液相氧化制备异丙苯过氧化氢的活性进行了研究。采用X射线衍射、傅里叶红外光谱、扫描电子显微镜和热分析等手段对Ca₄Cu _x Al-LDHs进行了表征,制备的Ca₄Cu _x Al-LDHs保留了水滑石的片层状结构,铜的掺杂使孔径变小,比表面积增大。当进料比（催化剂/异丙苯）为7.5 mg/mL,反应温度85 ℃,氧气流速为15 mL/min,反应时间7 h,异丙苯的转化率为34.5%,异丙苯过氧化氢的选择性为86.9%,催化剂循环使用5次后,异丙苯的转化率为31.2%,异丙苯过氧化氢的选择性为83.3%。研究为异丙苯过氧化氢开发了新的催化体系。     

Dielectric and Pyroelectric Properties of Compositionally Graded Pb(Zr1-xTix)O3 Thin Films Prepared by Sol-gel Process

"Compositionally graded ferroelectric lead zirconate titanate Pb(Zr1-xTix)O3 (PZT) thin films were grown on Pt/Ti/SiO2/Si substrates by using a sol-gel process. The final structure consists of six layers, up-graded graded films starting from PbZrO3 on the Pt electrode to the top PZT(50) layer, it consists of no Ti, 10%Ti, 20%Ti, 30%Ti, 40%Ti, and 50%Ti respectively. Whereas films with opposite gradient are called down-graded graded films. Structure and dielectric properties of the graded films was investigated by X-ray diffraction, Auger electron spectroscopy and by impedance analysis. The up-graded and down-graded PZT films annealed at 600 o, exhibited the remanent polarization values of 18.0 and 24.2 1C/cm2, respectively. The typical small signal dielectric constants and loss tanffi at a frequency of 100 Hz were 523 and 0.018, 544, and 0.020, respectively, for up-graded and down-graded PZT thin films. The temperature dependence of pyroelectric coeoients of the graded PZT films was measured by a dynamic technique. From 20 o to 82 o, the pyroelectric coeoients of the up-graded and down-graded PZT films up to 374 and 407 1C/m2K, respectively."     

Hydrothermal Preparation and Oxygen Storage Capacity of Nano CeO2-based Materials

"catalysts were synthesized by hydrothermal method. The X-ray diffraction result showed that the averageparticle size was in the range of 11-12 nm, which was correspondence to the high-resolution transmission electron microscopy result that the average particle size was about 12 nm. The specific surface area of the NiO-CeO2 binary compounds was in the range of 54-75 m2/g. Also the average particle size of the Bi2O3-CeO2 binary compounds was in the range of 8-11 nm. The oxygen storage capacity of the NiO-CeO2 and Bi2O3-CeO2 binary compounds was investigated under reduction and oxidation conditions. When the Ni and Bi concentration in CeO2 was up to 30%, the OSC values reached 2465 and 2560 1molO/g separately, which indicated that NiO and Bi2O3 compounded CeO2 materials have fine catalysis activity than other cations doped CeO2-based materials and appear to be very promising for practical applications such as OSC materials"     

三维有序金掺杂纳米TiO_2修饰电极用于抗肿瘤药物与DNA相互作用的研究

利用模板法在氧化铟锡(ITO)电极表面制备了三维有序多孔结构的金掺杂纳米Ti O2薄膜修饰电极(3DOM GTD/ITO),并在此修饰电极上成功固定小牛胸腺DNA(ct DNA),从而构建了一种新型的DNA生物传感器(DNA/3DOM GTD/ITO),并通过透射电镜(TEM)、扫描电镜(SEM)对修饰电极的表面形貌进行表征。采用电化学交流阻抗(EIS)法研究了ct DNA在3DOM GTD/ITO修饰电极表面的固定情况,结果表明,ct DNA已被成功地固定在3DOM GTD/ITO修饰电极表面。采用循环伏安法、微分脉冲伏安法等电化学方法研究了抗肿瘤药物槲皮素(Qu)在3DOM GTD/ITO修饰电极表面的电化学性质及与ct DNA的相互作用。结果表明,Qu在3DOM GTD/ITO修饰电极表面有1对准可逆的氧化还原峰,其氧化还原反应为2电子和2质子的转移过程。Qu可与固定在修饰电极上的ct DNA发生较强的结合作用,其结合常数(K)为3.61×106L/mol。循环伏安实验、紫外-可见吸收光谱、分子荧光光谱、圆二色性光谱均表明Qu与ct DNA之间的相互作用模式为嵌插作用。Qu与ct DNA的碱基结合具有序列选择性,对Qu与聚(d G-d C)及聚(d A-d T)的结合常数进行计算,得到结合常数比K(d G-d C)/K(d A-d T)=3.5,表明Qu与ct DNA发生嵌插作用时更倾向于结合在GC富集区域。     

三正辛胺络合萃取法分离提取糖果中8种合成色素

以三正辛胺为络合剂,四氯化碳为稀释剂,采用络合萃取法对糖果中的柠檬黄、新红、苋菜红、胭脂红、日落黄、诱惑红、亮蓝和赤藓红8种合成色素进行了预处理研究。考察了样品溶液p H值、稀释剂种类、三正辛胺浓度、反萃相组成等对预处理效果的影响。结果表明,当样品溶液p H值为6.0,以四氯化碳为稀释剂,三正辛胺浓度为5%,无水乙醇-15%氨水(体积比1∶1)为反萃相时,8种合成色素的回收率为90%~98%。该预处理方法操作简单、快速、有机溶剂用量少、回收率高,适用于糖果中多种合成色素的分离提取。     

催化动力学紫外吸光光度法直接测定水中痕量铜

以铜(Ⅱ)对过氧化氢氧化抗坏血酸的催化作用为基础,建立了一种催化动力学紫外吸光光度法直接测定水中痕量铜的方法。在pH3.5,0.0014mol·L-1抗坏血酸溶液,0.035mol·L-1过氧化氢溶液的体系中,方法的回收率为98.5%-99.4%,检出限为4μg·L-1。用以测定自来水、河水、生活污水中铜,结果满意。     

单层碳纳米管修饰电极上盐酸曲普利啶的电化学行为及其应用研究

应用循环伏安法研究了盐酸曲普利啶在碳纳米管修饰电极上的电化学行为.结果表明:在0.1 mol/L磷酸盐缓冲溶液(pH 6.9)中,盐酸曲普利啶产生一灵敏的氧化峰,其峰电位为0.81 V(vs.Ag/AgCl),峰电流与盐酸曲普利啶在1.0×10-6～1.3×10-4 mol/L浓度范围内呈线性关系,检出限为5.0×10-7mol/L,已用于片剂中盐酸曲普利啶的测定.     

Mg/Al物质的量比对Ce-La/MgAl2O4-x催化剂催化CO还原NO性能的影响

采用初始浸渍法制备了不同Mg/Al物质的量比的Ce-La/MgAl₂O₄-x催化剂,并通过低温N₂-吸附脱附、XRD、H₂-TPR和CO-TPR等手段对其进行了表征。结果表明,在Mg/Al物质的量比为0.5时,催化剂催化CO还原NO的性能最好。这主要是因为适量Mg的添加促进了CeO₂的分散和Ce-O-La固溶体的形成,从而使得表面Ce³⁺和氧空穴增加。两者的协同作用使得Ce-La/MgAl₂O₄-0.5表现出最佳的催化性能。另外,适量Mg的引入可以抑制Ce（SO₄）₂和Ce₂（SO₄）₃的形成,从而提高了Ce-La/MgAl₂O₄-0.5催化剂抗硫中毒能力。     

敞开式离子化质谱技术及其在微生物分析中的应用

敞开式离子化质谱(Ambient ionization mass spectrometry,AI-MS)是近年来兴起的质谱分析技术,可在敞开的大气环境下实现离子化,无需或只需少许样品前处理步骤,具有实时、简便、快速、高通量等诸多优点.近年来AI-MS技术的发展与应用已成为质谱领域备受关注的热点之一.该文综述了AI-MS...