毛细管电泳发光二极管诱导荧光对免疫球蛋白G的检测

采用自行设计、组装的毛细管电泳光导纤维发光二极管诱导荧光检测装置,建立了一种直接测定免疫球蛋白G(IgG)的方法。以蓝色发光二极管(LED)为荧光检测器的激发光源,荧光素异硫氰酸酯(FITC)为柱前衍生试剂,采用毛细管区带电泳,以20 mmol/L硼砂缓冲溶液(pH9.2)为背景电解液进行分离检测。通过对衍生反应条件和电泳分离条件进行优化,确定了最佳实验条件,在该条件下,IgG的线性范围为4.5×10-8~1.2×10-6g/L,检出限为2.0×10-8g/L。该方法简单、高效、选择性好,无需前处理,可用于人血清中IgG含量的测定。     

鱼腥草中钛含量分析方法研究

The research of the effects of surfactants on coloring reaction between titanium and phenyl fluorone was developed.A survey of coexisting elements in the houttuynia cordata thunb was carried out by X-ray fluorescence spectrometry,and a series of interference tests and analyses were performed.The interference can be eliminated by processing through high temperature cineration and adding ascorbic acid.A new method of determination of titanium in houttuynia cordata thunb was established by phenyl fluorone spectrophotometry in the presence of Emulsifier OP.The results showed that Beer's law is obeyed within the range of 0～0.32 μg·mL-1 for titanium.The relative standard deviation(RSD) was 1.9%～2.0%,and the recovery was 96.8%～100.6%.The method was applied for determination of titanium in houttuynia cordata thunb with satisfactory results.     

壬基酚聚氧乙烯醚型Gemini季铵盐表面活性剂的合成 及其表面性质的研究

合成了系列壬基酚聚氧乙烯醚型Gemini季铵盐表面活性剂(GNPQA), 用核磁、红外和元素分析对它们的结构进行了表征, 考察了反应条件对转化率的影响, 并用表面张力法和稳态荧光探针法对GNPQA的表面性能及胶束聚集数(N)进行了研究. 结果表明, 较优的反应条件: 反应时间为12 h, 反应温度为70 ℃, 反应原料摩尔比为n(双聚壬基酚聚氧乙烯醚)∶n(三乙胺)∶n(环氧氯丙烷)＝1∶1∶1; GNPQA的临界胶束浓度(CMC)值较相应的单体壬基酚聚氧乙烯醚型季铵盐表面活性剂(NPQA)降低了1～2个数量级, 显示了较高的表面活性; 当GNPQA溶液浓度为5～9倍CMC时, N值随浓度增大而线性增大; 随着氧乙烯(EO)单元数的增长, GNPQA的CMC和N值均逐渐减小; 结合GNPQA的表面性能参数和N值的变化规律, 探讨了这类表面活性剂表面及胶束聚集体的结构形态.     

邻菲咯啉合铜配合物与牛血清白蛋白的相互作用

利用荧光光谱法研究了两种配合物,[Cu（phen）（L-Phe）（H2O）]ClO4（1）（L-Phe为L-苯丙氨酸根）和[Cu（phen）（Gly）（H2O）]ClO4·2．5H2O（2）（Cly为甘氨酸根）,与牛血清白蛋白（BSA）的相互作用。结果表明,牛血清白蛋白的荧光强度随着配合物浓度的增大而逐渐降低,配合物（2）与BSA的结合常数大于配合物（1）与BSA的结合常数,牛血清白蛋白对配合物的结合位点数为1,荧光猝灭作用机理为静态猝灭．     

荧光共振能量转移测定牛血清白蛋白的研究

随着生物分析技术进入了后基因组时代,生命科学领域里的研究课题不断深入,DNA、RNA、蛋白质和其他生物大分子的检测技术发展十分迅速,生命科学中单分子分析技术不断揭示出生命活动的客观规律.相关的新的分析方法和仪器不断取得进展,成为生命科学的前沿领域.     

Syntheses, Crystal Structures and Fluorescence Properties of Two Triazolyl Derivatives with Biphenyl Links

Two novel triazolyl derivatives with biphenyl links, namely 4,4-bis（1,2,4-triazol-1-ylmethyl）biphenylene 1 and 4,4-bis（3,5-dimethyl-1,2,4-triazol-1-ylmethyl）biphenylene 2, have been synthesized and structurally characterized by single-crystal X-ray diffraction. Compounds 1·H2O·HCl and 2·2H2O·2HCl crystallize in the monoclinic system with space group C2/c and P21/c, respectively. The dihedral angles of the two phenyl rings are 30.26（6）° in 1·H2O·HCl, while co-planar （0.00（7）°） in 2·2H2O·2HCl. In 1·H2O·HCl, the N-H…O hydrogen bonds link 1 to form chain-like structures which are further connected by O-H…Cl, C-H…Cl, C-H…O and π-π supramolecular interactions. The hydrogen bonds of O-H…Cl in 2·2H2O·2HCl provide distinguishing P/M helical chains along the b axis, and these chains are further connected by N-H…O hydrogen bonds to generate a 2D structure. Compounds 1 and 2 in methanol solution show much stronger emission bands at 319 nm than biphenyl at 316 nm under excitation at 260 nm.     

微波灰化-氢化物发生-原子荧光光谱法测定原油和燃料油中的铅和砷

探讨了使用微波灰化技术消化原油和成品油样品,并使用氢化物发生-原子荧光光谱法测定其中铅和砷的含量.研究了铅测定的灰化保护剂和砷测定的灰化助剂,并优化了仪器工作条件和实验条件.该方法测定原油和重油中铅的平均回收率分别为96.8%和96.7%,相对标准偏差分别为1.03%和0.93%;测定原油和重油中砷的平均回收率分别为90.0%和90.3%,相对标准偏差分别为2.39%和2.63%.     

高效液相色谱-荧光检测法测定血清中的犬尿氨酸

建立了高效液相色谱-荧光检测(HPLC-FLD)测定血清中犬尿氨酸(kynurenine,Kyn)含量的方法。采用Hypersil C8色谱柱(300 mm×6.0 mm,10 μm), 流动相为0.25 mol/L醋酸锌及50 mmol/L醋酸溶液(含3%乙腈),流速为1.5 mL/min, 荧光检测激发波长和发射波长分别为365 nm和480 nm。血清标本经5%(v/v)高氯酸溶液去除蛋白质后取上层清液直接进样, Kyn经流动相等度洗脱分离后,用FLD进行测定。研究结果表明Kyn保留时间约为8.3 min,线性范围为0.098～19.6 μmol/L,最低检出浓度为0.04 μmol/L,回收率为90.8%～96.2%,日内、日间测定的相对标准偏差均小于5%,苯丙氨酸、酪氨酸、色氨酸、5-羟色胺和犬尿喹啉酸等物质对犬尿氨酸的测定均无干扰。建立的方法简便、快速、灵敏、特异,适用于临床和科研应用。     

腺苷与人血清白蛋白间相互作用的荧光光谱及分子模型法研究

在模拟人体生理条件下,结合紫外光谱和分子对接模型运用荧光光谱研究了腺苷与人血清白蛋白(HSA)间的键合作用。腺苷有较强的能力猝灭人血清白蛋白的内源荧光,且根据Stern-Volmer方程判断出猝灭机制为静态猝灭。本文运用相应的荧光值和Vant’Hoff热力学方程求得了不同温度下的结合常数(K)以及一些热力学参数,如焓变(ΔH)和熵变(ΔS)。结果表明：键合过程中疏水作用力对新化合物的稳定性起主要作用,这与分子对接模型方法研究的结果基本一致。另外还研究了常见离子对结合常数的影响。     

Synthesis,characterization, fluorescence and redox features of new <Emphasis Type="Italic">vic</Emphasis>-dioxime ligand bearing pyrene and its metal complexes

A new vic-dioxime ligand, N,N′-bis(aminopyreneglyoxime) (LH₂), and its copper(II), nickel(II) and cobalt(II) metal complexes were synthesized and characterized by elemental analyses, IR, UVVIS and ¹H and ¹³C NMR spectra (for the ligand). Mononuclear complexes were synthesized by a reaction of ligand (LH₂) and salts of Co(II), Ni(II), and Cu(II) in ethanol. The complexes have the metal-ligand ratio of 1: 2 and metals are coordinated by N,N′ atoms of vicinal dioximes. The ligand acts in a polydentate fashion bending through nitrogen atoms in the presence of a base, as do most vic-dioximes. Detection of a H-bonding in the Co(II), Ni(II), and Cu(II) complexes by IR revealed the square-planar MN₄ coordination of mononuclear complexes. Fluorescent properties of the ligand and its complexes arise from pyrene units conjugated with a vic-dioxime moiety. Fluorescence emission spectra of the ligand showed a drastic decrease in its fluorescence intensity upon metal binding. The electrochemical properties of the complexes were studied by the cyclic voltammetry technique. The nickel complex displayed an irreversible oxidation process while the copper complex exhibited a quasi-reversible oxidation and reduction processes based on the copper Cu(II)/Cu(III) and Cu(II)/Cu(I) couples, respectively.