粒径可控的纳米铁酸铋的制备及其光催化性能

采用改进的聚丙烯酰胺凝胶法制备了BiFeO3纳米颗粒,利用热重-差热、红外光谱及X射线衍射等手段研究了干凝胶的热分解及BiFeO3的成相过程.结果表明,在600℃煅烧可制备出高纯的BiFeO3纳米颗粒.同时发现,随着双丙烯酰胺含量的增加,所得样品晶粒尺寸逐渐减小,从而制备出平均粒径约52～110nm的系列BiFeO3颗...     

Synthesis and Characterization of a Homochrial Manganese（Ⅱ）Complex Constructed from （1R,2R）-（-）-Diaminocyclohexane-N,N biscarboxyl-salicylidene）

A homochrial manganese(Ⅱ) complex derived from chiral salen ligand (1R,2R)-(-)diaminocyclohexane-N,N-biscarboxyl-salicylidene) (1) has been synthesized through solvothermal procedure and characterized by IR,elemental analysis,TGA,circular dichroism (CD),powder and single-crystal X-ray crystallography.It crystallizes in monoclinic,space group C2 with a=32.987(7),b=7.4662(15),c=17.931(4),β=97.82(3)°,V=4375.0(15) 3,Z=8,D c=1.544 g/cm 3,F(000)=2096,M r=508.36,μ=0.658 mm-1,the final GOOF=0.975,R=0.0676 and wR=0.2068 for 6357 observed reflections with I > 2σ(Ⅰ).The coordination polymer 1 possesses a 1D infinite zigzag chain architecture constructed by the dicarboxyl-functionalized metallosalen ligand (MnSalen),and the polymeric chains are further assembled into a 2D supramolecular network structure via strong intermolecular hydrogen bonding interactions between the adjacent zigzag chains.     

Syntheses and Crystal Structures of Two Octamolybdate Compounds Modified by CuⅡ-Imidazole Cations

Two new polyoxomolybdate compounds,namely(CuIIL2)2[CuⅡ(HL)2]2[Mo8O26(HL)2].(H2O)4(1) and [CuⅡ(HL)2]2[β-Mo8O26](HL)2(2)(HL=imidazole),were designed and synthesized under hydrothermal conditions.X-ray diffraction analyses reveal that compound 1 consists of one Mo8O26(HL)24-cluster,two CuL2,two Cu(HL)22+,and four disassociated water molecules;and compound 2 is constructed by one β-Mo8O264-cluster,two Cu(HL)22+,and two uncoordinated imidazole molecules.     

N-(8-对氨基苯磺酰)胺基喹啉的合成及其荧光性质的研究

合成了一种Zn2+荧光探针N-(8-对氨基苯磺酰)胺基喹啉(HQAS),探讨了HQAS与Zn2+的键合比和配位模式,以及不同pH,其它金属离子对Zn2+检测的影响.研究结果显示:该探针与Zn2+形成配合物,使其荧光增强,键合比为2:1,pH 7.2时荧光强度增大9.4倍.大多数金属离子几乎不干扰Zn2+的检测,Cu2+...     

应用光亲和分子进行PEG的光照修饰及蛋白质的光照偶联

合成了一种光活性标记分子-对叠氮苯甲酸,将其偶联到具有双羟基的碳酸酯与乳酸的共聚物P (LA-co-DHP)上,获得了具有光反应活性的可生物降解共聚物P(LA-co-DAP),在光照条件下,可以将蛋白质方便快捷地共价偶联到P(LA-co-DHP)聚合物纤维上.在溶液中进行PEG与对叠氮苯甲酸的光照反应,通过核磁共振光谱...     

气相色谱-质谱法测定电子产品中四溴双酚A

建立了超声提取-硅烷化气相色谱-质谱测定电子产品中四溴双酚A的方法.样品用正己烷/丙酮作提取剂,浸泡后超声提取,经N,O-双三甲基硅烷三氟乙酰胺(BSTFA)+1%三甲基氯硅烷(TMCS)衍生化,利用气相色谱-质谱仪进行定性定量分析.讨论了浸泡时间对提取效率的影响,优化衍生温度和衍生时间.结果表明:标样衍生后在0.4～...     

脯氨酸与Ag和Ag+相互作用及性质

用X3LYP杂化密度泛函方法在LACV3P^**++基组水平上对脯氨酸(Pro)的15种构象与Ag原子和Ag⁺离子形成多种配合物的几何结构、电子结构、振转光谱和能量学特征进行了计算研究, 结果得到17种Pro-Ag和23种Pro-Ag⁺稳定结构. 数据分析表明: (1) Pro-Ag配合物中仅有Pro的9种构象出现, 而Pro-Ag⁺配合物中则都涉及, 最稳定结构并不是能量最低的Pro构象与Ag或Ag⁺生成; (2) Pro与4d¹⁰5s¹组态的Ag结合主要是范德华作用力, 对Pro结构影响很小, 配合物中存在较弱的特殊O―H…Ag氢键. 外层5s5p全空的Ag⁺与配位原子间生成σ配位键. 前者以单配位最稳定, 后者以双配位最稳定; (3) Ag原子与Pro配位结合能小于-19 kJ·mol^-1, 而Ag⁺与Pro的结合能在-117 - -255 kJ·mol^-1范围, 形成热力学稳定体系Pro-Ag⁺; (4) 自然键轨道(NBO)布局分析显示 Pro-Ag和Pro-Ag⁺体系中Ag都获得少量负电荷, 配合物的前线轨道能量差(Δε)均比两个碎片的低. 配合物中O―H和N―H键的红移和蓝移都存在.     

Total syntheses of drimane-type sesquiterpenoids enabled by a gold-catalyzed tandem reaction

Development of a gold-catalyzed tandem reaction of 1,7-diynes with both internal and external nucleophiles was realized, which constructed five chemical bonds, two rings, and two stereogenic centers in a single step. Based on the novel cascade transformation, we achieved a unified strategy toward the stereoselective total syntheses of C-15 oxygenated drimane-type sesquiterpenoids and their analogues, which provided the natural products kuehneromycin A, antrocin, anhydromarasmone, and marasmene as a proof-of-concept study.     

高效液相色谱-电喷雾离子阱串联质谱法检测芥子气经皮肤染毒SD大鼠肺中的DNA加合物

运用高效液相色谱-电喷雾离子阱串联质谱(HPLC-ESI-MS/MS)技术,建立了快速、简单、灵敏的SD大鼠肺中N7-(2-羟乙基硫代乙基)鸟嘌呤(N7-HETEG)的检测方法。以N7-苯甲基鸟嘌呤为内标,用甲醇和水为流动相进行梯度洗脱,正离子模式检测,方法的检出限(信噪比(S/N)≥10)为300 pg/mL,定量限(S/N≥20)为850 pg/mL。在300 pg/mL～1.28 μg/mL的质量浓度范围内,N7-HETEG浓度与N7-HETEG和内标的峰面积比呈良好的线性关系(线性相关系数为0.9929)。高、中、低3个添加水平的日内测定精密度(以相对标准偏差(RSD)计)和日间测定精密度均小于10%(n=7),回收率为100%～132%。对SD大鼠背部皮肤染芥子气,剂量分别为5.5、11、22和45 mg/kg,染毒4 d后检测大鼠肺脏中N7-HETEG的含量。各个不同染毒剂量下,每克组织中分别检测到（0.56±0.16）、（0.67±0.12）、（1.36±0.68）和(5.14±0.92) ng N7-HETEG, N7-HETEG的含量随着染毒剂量的增大而增大,表明N7-HETEG可用作芥子气暴露的体内生物标志物。