手性二茂铁色氨酸化合物[Fc-(CO-L-Trp-OMe)2]的合成和结构表征

由色氨酸甲酯和1,1′-二茂铁二羧酸合成了化合物1[Fc-(CO-L-Trp-OMe)₂],并对化合物1在固体和溶液中的结构进行了表征。单晶结构表明,该化合物通过2个分子内氢键,形成了规则的手性构象。通过分子间的氢键,形成了二维网状结构。对化合物1的乙腈溶液进行了CD谱的测定,结果表明,该化合物在溶液中呈现P螺旋构象。¹H NMR谱和FTIR谱也证实了该化合物在固体和溶液状态中都形成了含分子内氢键的构象。     

Determination of the migration of fourteen endocrine disruptors in food packaging materials by liquid chromatography-tandem mass spectrometryEI北大核心CSCD

A method for the determination of the migration of 14 endocrine disruptors（bisphenol A,bisphenol E,bisphenol F,bisphenol S,bisphenol B,bisphenol Z,bisphenol AF,bisphenol AP,tetrabromobisphenol A, tetrachlorobisphenol A,octylphenol,4-n-octylphenol,4-nonylphenol and 4-n-nonylphenol）in food packaging materials by liquid chromatography-tandem mass spectrometry was developed. The samples were soaked in water,4% acetic acid solution,10% ethanol solution,50% ethanol solution,olive oil,simulated sweat and simulated saliva. The soakings were purified by solvent extraction or Oasis HLB solid phase extraction. After separation by a Waters Atlantis™ T3 column,the samples were determined by multiple reaction monitoring mode with electrospray negative ion source,and quantified by matrix external standard method. The linear correlation coefficients of 14 endocrine disruptors were 0.9901-0.9986,the recoveries were 82.3%-108.7% with the relative standard deviations of 0.8%-6.8%,the limits of detection were 0.1-0.5 μµg/L and the limits of quantification were 0.3-1.5 μµg/L. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

固相萃取-液相色谱-串联质谱法测定儿童消费品中14种酚类物质的迁移量

儿童通过手、口等途径接触儿童消费品时,双酚A等酚类物质会通过唾液或汗液迁移到体内,影响儿童健康,而关于唾液和汗液中酚类物质迁移量检测的报道较少,因此进行了题示研究。将样品剪碎或粉碎成粒径小于2mm的颗粒,分取1.00g,加入20mL模拟汗液或模拟唾液,浸泡2.0h后分取10mL过活化好的Oasis HLB固相萃取柱,用5mL水淋洗,8mL甲醇洗脱。收集洗脱液,氮吹至近干,用30%(体积分数)甲醇溶液稀释至2.0mL,过0.22μm滤膜。滤液进入液相色谱-串联质谱仪,目标物在AtlantisTMT3色谱柱上以不同体积比的水和体积比1∶1的甲醇-乙腈混合溶液进行梯度洗脱分离,以电喷雾离子源负离子模式电离,以多反应监测模式检测,以基质匹配法定量。结果显示：14种酚类物质的质量浓度分别在0.1～20.0μg·L^-1(双酚A、双酚AF和四氯双酚A)和0.5～100.0μg·L^-1(其他11种酚类物质)内与峰面积呈线性关系,检出限(3S/N)为0.3～1.5μg·kg^-1。按标准加入法进行回收试验,模拟汗液和模拟唾液中14种酚类物质...     

钴、碳共掺杂氮化碳的制备及其光催化分解水产氢性能

针对氮化碳可见光利用率低和在光催化过程中光生电子与空穴易于复合的缺点,通过钴、碳共掺杂提升其光催化性能。以尿素为前驱体,维生素B12（VB12）为钴源和碳源,将二者的混合物进行一步煅烧,制备钴、碳共掺杂氮化碳（CNCoC）。结果表明,钴、碳共掺杂对氮化碳的微观形貌、骨架结构和官能团都没有造成明显影响;但是增大了产物的比表面积,调节了产物的能带结构,增加了其对可见光的吸收。更重要的是,相比于单一元素碳的掺杂,钴、碳共掺杂具有协同作用,能够更有效地提升光生电子和空穴的分离和传递效率。因此,加入6 mg VB12制备的CNCoC-6的可见光光催化分解水产氢速率达到了56.1 μmol·h^-1,是纯氮化碳（CN）的3.05倍;而碳掺杂氮化碳（CNC-6）的产氢速率仅为CN的2.55倍。     

Electric gating of the multichannel conduction in LaAlO_3/SrTiO_3 superlattices

The electric gating on the transport properties of two-dimensional electron gas(2DEG) at the interface of LaAlO₃/SrTiO₃(LAO/STO) heterostructure has attracted great research interest due to its potential application in fieldeffect devices. Most of previous works of gate effect were focused on the LAO/STO heterostructure containing only one conductive interface. Here, we systematically investigated the gate effect on high-quality LAO/STO superlattices(SLs)fabricated on the TiO₂-terminated(001) STO substrates. In addition to the good metallicity of all SLs, we found that there are two types of charge carriers, the majority carriers and the minority carriers, coexisting in the SLs. The sheet resistance of the SLs with a fixed thickness of the LAO layer increases monotonically as the thickness of the STO layer increases. This is derived from the dependence of the minority carrier density on the thickness of STO. Unlike the LAO/STO heterostructure in which minority and majority carriers are simultaneously modulated by the gate effect, the minority carriers in the SLs can be tuned more significantly by the electric gating while the density of majority carriers is almost invariable. Thus, we consider that the minority carriers may mainly exist in the first interface near the STO substrate that is more sensitive to the back-gate voltage, and the majority carriers exist in the post-deposited STO layers. The SL structure provides the space separation for the multichannel conduction in the 2 DEG, which opens an avenue for the design of field-effect devices based on LAO/STO heterostructure.     

不同波长飞秒脉冲的相位测量

飞秒脉冲技术的不断发展能够较方便地产生不同波段和结构特性的飞秒脉冲. 对已有的改进型零附加相位光谱相位相干电场重构系统进行优化整合,使之胜任不同特性飞秒脉冲的测量. 利用该系统测量了两台飞秒激光系统输出不同波长的脉冲及其通过厚度为80 mm的BK7玻璃块而得到的啁啾脉冲. 实验结果表明,该系统的适用范围较宽. 关键词： 光谱相位相干直接电场重构法 飞秒脉冲测量 波长     

核壳结构磁性镁铝复合氧化物亚微米粒子的制备与表征

首先采用溶剂热法制备粒径均匀分散性良好的Fe3O4亚微米粒子,在对其包覆上一层碳膜进行表面修饰后,采用共沉淀法将硝酸根插层LDHs包覆到磁性粒子的表面,然后500℃焙烧2 h得到磁性镁铝复合氧化物亚微米粒子。这种磁性镁铝复合氧化物亚微米粒子具有以镁铝复合氧化物为壳层,Fe3O4为核的核壳结构,其中壳层厚度为20 nm左右,对其进行二次包覆后壳层厚度可达到50 nm左右,并可以方便的通过重复包覆焙烧过程进行调节,从而实现磁性镁铝复合氧化物亚微米粒子的控制制备。同时,磁性镁铝复合氧化物亚微米粒子具有较强的磁性,其比饱和磁化强度为23.3 emu·g-1,对其进行二次包覆并焙烧后为20.1 emu·g-1。     

Fe2O3与TiF3添加剂对LiBH4-MgH2复合氢化物体系的协同催化作用

通过球磨方法制备出2LiBH4-MgH2,2LiBH4-MgH2-10%Fe2O3,2LiBH4-MgH2-10%TiF3,2LiBH4-MgH2-5%Fe2O3-5%TiF3和2LiBH4-MgH2-10%Fe2O3-10%TiF35个复合氢化物体系,用热重(TG)、差示扫描量热(DSC)、X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)和压力-组成-温度仪(PCT)等对所制备体系进行表征.结果表明,Fe2O3和TiF3的掺杂均能够有效地改善2LiBH4-MgH2复合体系的放氢性能,尤其是两者共掺杂的2LiBH4-MgH2-10%Fe2O3-10%TiF3体系,初始放氢温度为110℃,总放氢量达到约9.6%.对2LiBH4-MgH2-5%Fe2O3-5%TiF3体系的PCT表征结果表明,在400℃时,10 min内放氢量达到了8.6%,放氢热力学和放氢动力学均优于单一相的掺杂,体现了两相掺杂的协同催化作用.     

微波灰化-氢化物发生-原子荧光光谱法测定出口小麦淀粉中痕量铅

建立了微波灰化,断续流动-氢化物发生-双道原子荧光光度计测定小麦淀粉中痕量铅的方法,解决了小麦淀粉前处理难的问题,研究了加入硝酸后对铅测定的影响,探讨了酸度、还原剂浓度、基体效应对氢化物发生的影响。铅的线性范围为1.00-200.0μg/L,方法检出限为0.57μg/L,回收率为88.50%-103.3%,精密度为2.54%-4.82%。     

俾士麦棕与核酸相互作用的吸收光谱行为

利用分光光度法研究了俾士麦棕与核酸的结合作用。当pH在6．9—7．6时,体系在446nm处有最大吸收峰,且在室温下2min达到稳定且吸光度在3h之内保持不变。在最佳显色条件下,小牛胸腺脱氧核糖核酸（et DNA）和鲱鱼脱氧核糖核酸（fs DNA）的线性范围分别为0．1—18mg／L和0．1～28mg／L;检出限分别为0．019mg／L和0．028mg／L。采用摩尔比法和Rosenthanl作图法测定了俾士麦棕与核酸的结合数,且利用Rosenthanl作图法获得了俾士麦棕与核酸的结合常数。两种方法所得结合数基本一致,即核酸分子中的一个核苷酸可与3个染料分子结合。该方法灵敏度高,稳定性好,操作简便,重现性好以及抗干扰能力强,用于合成样品的分析,回收率在95．2％-102％之间;相对标准偏差低于4．9％,结果令人满意。