废水中类固醇物质的LCMSMS检测方法优化及其在养殖废水检测中的应用

以固相萃取为预处理手段,用高效液相色谱-串联四极杆质谱联用技术,针对澳大利亚南威尔士州畜牧业废水中的丙酸睾酮等13种类固醇化合物含量建立了分析方法.采用大气压化学电离源,在正离子模式下,对色谱条件和质谱条件进行优化,其中,丙酸睾酮等7种化合物以质子化的准分子离子峰[M+H]+、另6种化合物以产生了脱去水的离子峰[M+H-H2O]+为母离子进行二级质谱扫描,以最大丰度确定定量离子对.结果表明:该方法所建立的13种化合物的9点标准曲线的线性相关范围为1～1000ng·ml-1,在该范围内,相关系数均>0.9990;各化合物的平均回收率在83.75%～111.50%,相对标准差2.02%～14.21%;除美雌醇和雌三醇的灵敏度相对较低,检测限高于15ng·ml-1外,其余物质的检测限均低于5ng·ml-1;实际样品测定时,不同处理流程中各化合物的浓度均能得到较好体现,该方法能满足检测要求.

国产12种苔藓植物的染色体数目

报道了中国产 1 2种苔藓植物染色体数目 ,结果为 :壶苞苔Blasiapusilla ,n =9;艳绿光苔Cy athodiumsmaragdinum ,n =9;紫背苔Plagiochasmarupestre,n =9;石地钱Rebouliahemisphaerica ,n =9;宽片叶苔Riccardialatifrons,n =1 0 ;尖叶美喙藓Eurhynchiumeustegium ,n =1 1 ;东亚沼羽藓Helodiumsachali nense,n =1 1 ;白齿藓Leucodonsciuroides,n =1 1 ;齿边细枝藓Lindbergiaserrulatus,n =1 1 ;疣小金发藓Pogonatumurnigerum ,n =7;台湾拟金发藓Polytrichastrumformosum ,n =7;金发藓Polytrichumcommune,n=7。其中艳绿光苔、齿边细枝藓和东亚沼羽藓的染色体数目为首次报道。

水肥耦合对春小麦水分利用效率的影响

采用312-D最优饱和设计,在辽西半干旱区开展了连续4年的春小麦田间水肥耦合试验,研究春小麦水分利用效率。结果表明:水肥单因子对水分利用效率有显著影响,影响顺序为:水>磷>氮。其中,氮、磷施用量对水分利用效率的提高是正效应,而灌水量对水分利用效率是负效应。水肥多因子对水分利用效率有交互效应,氮与磷之间、氮与水之间的交互效应极显著,对水分利用效率表现为正效应。磷与水之间表现为负效应,但不显著。水分利用效率超过10kg/(hm2·mm)的水肥优化管理方案为,施氮量102 6～239 3kg/hm2,施磷量84 3～139 0kg/hm2,灌水量41 0～170 9mm。获得最大水分利用效率的施氮量220 6kg/hm2,施磷量76 0kg/hm2,灌水量117 4mm。

汶川5.12大地震地表次生灾害评价与分析

针对汶川5.12大地震,对由地震引起的地质次生灾害发生的坡度和坡向进行了统计,分析了地表破坏的易发坡度、坡向及其与震中的关系等。另外,分别以不同震中距为缓冲区、以平行中央断裂带的各级缓冲区、以等烈度区为缓冲区对地震引起的地表破坏的空间分布以及发生地表破坏的坡度在各级缓冲区中的变化进行了分析。结果表明:①地震引发的滑坡及滑坡群共5093个,总面积大约958km2;②在30°～44°坡度区间地表破坏发生的数量最大,42°坡度为地表破坏发生概率的拐点。主要的地表破坏发生在迎着地震波传播的坡向上;③随着震中距的增

Microstructure and mechanical properties of Mg-12.3Zn-5.8Y-1.4Al alloy

Microstructure and mechanical properties of as-cast and heat-treated Mg-12.3Zn-5.8Y-1.4Al (ZYA1261) alloy were investigated. The phase compositions of the as-cast alloy are alpha-Mg, Mg3YZn6 (I-phase), Mg(3)y(2)Zn(3) (W-phase), Mg12YZn (Z-phase), Mg24Y5, MgZn and a small quantity of Al-containing phase.

1.54 mu m near-infrared photoluminescent and electroluminescent properties of a new Erbium (111) organic complex

The crystal structure of Er(PM)(3)(TP)(2) [PM = 1-Phenyl-3-methyl-4-isobutyryl-5-pyrazoloiie, TP = triphenyl phosphine oxide] was reported and its photoluminescence properties were studied by UV-vis absorption, excited, and emission spectra. The Judd-ofelt theory was introduced to calculate the radiative transition rate and the radiative decay time of 3.65 ms for the I-4(13/2) -> I-4(15/2) transition of Er3+ ion in this complex.

In Situ Scanning Tunneling Microscopy on the Dynamic Process of the Replacement of Coronene on Au (111) by 6-Mercapto-1-Hexanol

The replacement of coronene monolayer on Au (111) by 6-mercapto-1-hexanol (MHO) was studied by in situ scanning tunneling microscopy (STM) in solutions. It was found that the rate of replacement depends strongly on the concentration of MHO. The replacement finished within a second at a higher concentration of MHO. At a lower concentration, the slow replacement could be followed by in situ STM. The replacement occurred initially near the elbow position of reconstructed Au (111) with the formation of pits in a single or several missing molecules. With the proceeding of replacement, these small pits expanded, and the surrounding coronene molecules were gradually substituted by MHO, which developed into ordered domains within a spatial confined environment. Meanwhile, the reconstruction of Au (111) was lifted. The replacement expanded fast along the reconstruction lines in the domain. For the fast replacement, a (root 3 x root 3) R30 degrees adlattice was observed, while a c(4 x 2) superlattice was observed for the slow replacement.

碱基腺嘌呤与胸腺嘧啶在Au(111)电极上的共吸附

用循环伏安法(CV)和电化学扫描隧道显微镜(ECSTM)在HClO4溶液中研究了配对碱基腺嘌呤(Adenine,A)与胸腺嘧啶(Thymine,T)在Au(111)电极上的共吸附行为。CV曲线表明,A和T的电化学共吸附行为更接近于A的电化学吸附行为。高分辨STM图像显示,在物理吸附区域碱基A和T分子之间通过氢键作用形成一种不同于单组分的网络结构。根据STM图像提出一个可能的模型,并给出了在Au(111)电极上共吸附时A和T分子之间可能的氢键作用方式。

Surface enhanced Raman scattering of brilliant green on ag nanoparticles and applications in living cells as optical probes

In this article, surface enhanced Raman scattering (SERS) of different concentrations of brilliant green (13G) on Ag nanoparticles (AgNPs) has been investigated. The results indicate that only 10(-12) M BG can be detected on AgNPs while as low as 10(-11) M BG can be detected upon the activation of AgNPs by chloride ions. The additional improvement of the detection of BG mainly derives from the increase of the electromagnetic field around AgNPs and partially from the reorientation of BG on AgNPs induced by chloride ions, which was proved by the different spectra feature in the two systems. Adsorption of BG on AgNPs has also been demonstrated in applications of living cells as optical probes based on SERS, indicating that dye-AgNPs can probe the local environment in the living cells. The related cytotoxicity measurements demonstrated that BG-AgNPs produced little cytotoxicity to the cells, which shows great potential in biornedical applications of BG labeled-AgNPs for SERS nanosensors in cells as optical probes. Meanwhile, SERS spectra of BG on AgNPs in the presence chloride ions are expected to be used in living cells as more sensitive optical probes.

Assembly of 12-tungstosilicic acid and 4-aminobenzo-15-crown-5 ether based on the electrostatic attraction through bridging of oxonium ions on different substrates

Based on the electrostatic attraction Keggin-type polyoxometalate H4SiW12O40 (SiW12) and small molecule 4-aminobenzo-15-crown-5 ether (4-AB15C5) were alternately deposited on poly (allylamine hydrochloride) (PAH)-derived indium tin oxide (ITO) substrate through a layer-by-layer (LBL) self-assembly, forming a supramolecular multilayer film (film-A). SiW12 was also deposited on a glassy carbon electrode (GCE) derived by 4-AB15C5 via covalent bonding in 0.1 M NaCl aqueous solution and formed a composite monolayer film (film-B). UV-vis absorption spectroscopy, X-ray photoelectron spectroscopy (XPS) and Fourier-transform infrared (FTIR) spectroscopy measurements demonstrated that the interactions between SiW12 and 4-AB15C5 in both two film electrodes were the same and caused by the bridging action of oxonium ions. But, the nanostructure in the two film electrodes was different. 4-AB15C5 in film-A was oriented horizontally to ITO substrate, however, that in film-B was oriented vertically to GCE. Namely film-A corresponded to a layer structure, and film-B corresponded to an intercalation structure.

Surface enhanced Raman scattering of brilliant green on ag nanoparticles and applications in living cells as optical probes

In this article, surface enhanced Raman scattering (SERS) of different concentrations of brilliant green (13G) on Ag nanoparticles (AgNPs) has been investigated. The results indicate that only 10(-12) M BG can be detected on AgNPs while as low as 10(-11) M BG can be detected upon the activation of AgNPs by chloride ions. The additional improvement of the detection of BG mainly derives from the increase of the electromagnetic field around AgNPs and partially from the reorientation of BG on AgNPs induced by chloride ions, which was proved by the different spectra feature in the two systems. Adsorption of BG on AgNPs has also been demonstrated in applications of living cells as optical probes based on SERS, indicating that dye-AgNPs can probe the local environment in the living cells. The related cytotoxicity measurements demonstrated that BG-AgNPs produced little cytotoxicity to the cells, which shows great potential in biornedical applications of BG labeled-AgNPs for SERS nanosensors in cells as optical probes. Meanwhile, SERS spectra of BG on AgNPs in the presence chloride ions are expected to be used in living cells as more sensitive optical probes.

硅（111）和金（111）基底自组装膜表面纳米图案化与功能化

利用导电原子力显微镜在烷基化自组膜/Si(111)和巯基自组膜/Au(111)上加工纳米模板,结合组装的方法构建功能化纳米图案。在烷基化自组膜/Si(111)上施加偏压可以得到SiO2纳米图案,此图案可以做功能化模板,将图案化区域组装胺基作为端基的硅烷后,通过1-乙基-3-（3-二甲基氨基丙基）碳二亚胺盐酸盐(EDC)/N-羟基琥珀酰亚胺(NHS)试剂活化共价结合11-巯基十一酸(MUA)稳定的金纳米粒子,得到金纳米粒子功能化纳米图案。在烷基硫醇自组装膜/Au(111)施加偏压可以选择性移除自组装膜,移除自组装膜后新暴露的金可以用做纳米模板,在此模板上组装MUA后通过EDC/NHS活化共价键合溶菌酶,得到蛋白质功能化的纳米点阵图案。

Large-scale, uniform DNA network on 11-mercaptoundecanoic acid modified gold (111) surface: Atomic force microscopy study

Large-scale, uniform plasmid deoxyribonucleic acid (DNA) network has been successfully constructed on 11-mercaptoundecanoic acid modified gold (111) surface using a self-assembly technique. The effect of DNA concentration on the characteristics of the DNA network was investigated by atomic force microscopy. It was found that the size of meshes and the height of fibers in the DNA network could be controlled by varying the concentration of DNA with a constant time of assembly of 24 h.