一种用于测定F~-的比色和荧光增强型探针

本文利用F~-诱导Si-O键断裂原理,以亚胺香豆素为荧光母体,成功合成了一种比色和荧光增强型F~-探针。由于探针分子结构的自由度较大,探针分子在乙腈溶液中几乎没有荧光,但随着F~-的加入探针分子经历Si-O键断裂及成环反应,生成具有较大共轭结构的环化产物,其荧光光谱在452nm处呈现出显著的荧光峰(荧光增强46倍),溶液的最大吸收峰由315nm红移至410nm(红移95nm),溶液的颜色由无色变为黄色,适用于裸眼检测F~-。同时,相对于其他阴离子(Cl~-、Br~-、I~-、NO_3~-、HSO_4~-、ClO_4~-、Ac~-、H_2PO_4~-),探针分子表现出对F~-较高的选择性和专一性,为F~-浓度的监测提供了一种高效灵敏的分析方法。     

Cu-MOF催化过氧化氢应用于多巴胺的检测

本文利用一种具有H_2O_2催化活性的Cu-MOF[Cu_3(BTC)_2(H_2O)_3,简称HKUST-1],构建了以邻苯二胺(OPD)为颜色指示分子的比色传感体系,实现了对H_2O_2和多巴胺(DA)的快速灵敏检测。HKUST-1起到催化H_2O_2氧化OPD的作用,反应体系能够呈现出显著的颜色变化。在优化条件下,415nm处的吸收峰强度与H_2O_2浓度呈双线性关系,线性范围分别为10~50 mmol/L和50~100 mmol/L,相对标准偏差分别为0.9947和0.9995,最低检出限为1.29mmol/L。由于DA能抑制H_2O_2氧化OPD,因此比色传感体系还可以用于快速检测DA,线性范围分别为0.25~5μmol/L和2.5~25μmol/L,相对标准偏差分别为0.9783和0.9705,最低检出限为0.262μmol/L。该项工作拓展了Cu-MOFs材料在生物分子催化和生物传感方面的应用。     

基于分子内电荷转移的阴离子比率荧光分子探针

设计合成了一种基于4-甲基-1-羟基二苯甲酮对硝基苯腙的比色和比率荧光阴离子受体1。此类受体以羟基和腙单元为识别位点,以硝基苯基为信号报告基团。向受体1的DMSO溶液中加入AcO-、H2PO4-、F-后,溶液颜色由黄色变为紫红色,而加入所研究的其它阴离子则无变化,从而实现对AcO-、H2PO4-、F-这三种离子的裸眼识别。利用紫外-可见吸收光谱、荧光光谱考察了其与AcO-,H2PO4-,F-,Cl-,Br-,I-等阴离子的识别作用。1H NMR滴定为受体分子与阴离子之间氢键作用本质提供了有力证据。     

Study on Cyclometalated Palladium-azo Complexes as Colorimetric Probes for Hazardous Gas in Water

A synthesized cyclometalated palladium-azo complex was explored as a multifunctional probe for visual detection of SO2, H2S and NH3 in water. In acidic aqueous environment, the sensing solution underwent a sharp color change from poor violet to deep blue when titrated with Na2SO3 standard solution. But the color changed from poor violet to bright yellow when titrated with Na2S standard solution. In basic environment, the sensing solution rapidly changed to magenta when titrated by NH4Cl-NH3 standard buffer solution at high concentration. However, the color of sensing solution changed to blue when titrated by NH4Cl-NH3 standard buffer solution at low concentration although the pH was kept constant during the titration. Different species of these hazardous gases at environmentally relevant concentration levels were differentiated by independent optical signal outputs, and the interference from other inorganic ions commonly existing in water was very small.     

微波溶样纳氏比色法测定食品中蛋白质

采用微波溶样技术消解食品样品，用纳氏比色法测定食品中蛋白质。实验结果表明，用微波溶样技术消解食品具有节省时间、节约试剂、消解完全等优点。本方法的相对标准偏差为0．4％－5．3％；回收率为95．0％－102．0％。     

基于次血红素六肽的过氧化氢和葡萄糖灵敏比色方法

采用次血红素六肽(DhHP-6)催化H₂O₂氧化4-氨基安替吡啉-氯代苯酚显色体系,建立了测定H₂O₂和葡萄糖的方法。 研究了pH值、底物浓度和DhHP-6浓度对实验的影响,检测了比色方法的反应线性、稳定性、相关性和回收率。 在最佳反应条件下,DhHP-6在不同时间及温度条件下,活性要优于过氧化物酶(POD);DhHP-6催化H₂O₂ 的米氏常数(K_m)和最大反应速率(v_max)分别为0.171 mmo/L和4.22×10^-6 mol/s;H₂O₂响应的线性范围为0.39~25.0 mmol/L;高、中、低 3水平测定的变异系数(CV)和加标回收率分别在1.29%~2.16%和94.5%~101.1%之间;与葡萄糖商品试剂盒比较相关系数R²=0.9946;36例血液样品中的葡萄糖浓度在4.26~17.48 mmol/L之间。 与葡萄糖检测商品试剂盒之间的两组数据经统计差异不显著(P>0.05)。 该方法是一种简单、廉价、方便、灵敏的比色测定方法。     

偶氮苯基型离子液体溶液对空气中湿度的变色响应

Room temperature ionic liquids (ILs) that can exhibit a colorimetric response to moisture in the air are rarely reported in the literature. In this study, an azophenolic IL solution exhibited a spontaneous a colorimetric response, driven by the formation of hydrogen bonding between the [PhN＝NPhO] anion and moisture in the air. This phenomenon was clearly understood using ultraviolet-visible (UV-Vis) absorption spectroscopy, nuclear magnetic resonance (NMR) spectra, experimental data, and theoretical calculations. Specifically, in the UV-Vis absorption spectra, absorption around 455 nm decreased, while the band around 343 nm increased in the IL CHCl₃ solution as time progressed; this was accompanied by a color change from orange to faint yellow. This spontaneous, self-responsive process was further observed using ¹H NMR data. When the IL solution was placed with sufficient time, all the ¹H NMR peaks of the azophenolic anion shifted downfield, but no new signals appeared in the upfield region. The reason for this was easily identified as the stimuli in the air, such as CO₂ and moisture. When pure CO₂ was bubbled through the IL CHCl₃ solution, the solution color changed from its original orange to light orange, but could not change further to faint yellow, which ruled out CO₂ gas as a stimulus. When a small amount of water was gradually added to the IL solution (MeCN solvent), the absorption band around 474 nm decreased, coupled with an increase in the absorption band around 347 nm. This was accompanied by a color change from orange to faint yellow, which was almost identical to the self-responsive process in CHCl₃ and CCl₄. Moreover, two cuvettes of IL CHCl₃ solution were placed under relative humidities of 28% and 100%, respectively; the IL CHCl₃ solution required a much longer time to exhibit a complete color change from orange to faint yellow under a lower relative humidity, demonstrating that moisture is the most likely stimulus triggering the self-responsive color change of the IL solution. As revealed by the Gaussian 09 program at the B3LYP/6-31++G(p, d) level, the distance between the oxygen atom on the azophenolic anion and the hydrogen atom on the H₂O molecule was 0.174 nm, and the corresponding angle was 171.12°. Furthermore, the atomic dipole moment corrected Hirshfeld (ADCH) charge of the oxygen atom on the azophenolic anion was −0.52, and it increased to −0.62 after the azophenolic anion interacted with the H₂O. Reduced density gradient analysis revealed that the spike corresponding to O∙∙∙H―O for the IL-H₂O complex was located at around −0.04 a.u.. All the above data indicate that the presence of hydrogen bonding rendered the IL solution responsive to the moisture stimulus, and this response was accompanied by a color change that was visible to the naked eye. To the best of our knowledge, this is the first demonstration of a colorimetric change in an IL solution in response to moisture. We hope this work can help us to gain insight into some seemingly abnormal phenomena that occur during the research process.     

纳米光学传感器用于检测汞离子

汞离子是毒性最大的重金属之一,对环境和人体都会造成严重的不良影响,开发能够快速检测环境中汞离子的分析方法引起了越来越多的关注。纳米材料由于其优良的光学性能和良好的稳定性,被广泛用于环境中汞离子的检测。本文主要综述了近年来一些代表性的基于纳米材料的汞离子荧光、比色传感器。根据纳米材料的不同,将这些传感器分为基于金、银、碳和硅基材料,以及量子点、有机纳米颗粒和其他纳米基材料的荧光、比色传感器,并分别从设计原理、识别性能和实际应用等方面对这些传感器进行了描述和讨论。最后对该领域的研究和发展提出了展望。     

基于没食子酸和对硝基酚双功能化银纳米粒子检测水中Cr3+

采用硼氢化钠还原法合成没食子酸和对硝基苯酚双功能化的银纳米粒子（GA-PNP-AgNPs）,并通过紫外-可见光谱法、透射电子显微镜和粒度仪对合成的银纳米粒子进行了表征。GA-PNP-AgNPs呈分散的球形,粒径约为21 nm,且在390 nm处有一个特征吸收峰。当Cr3+存在时,GA-PNP-AgNPs发生聚集,溶液颜色由淡黄色变为橙红色。基于此,构建了一种检测Cr3+的比色传感器,线性范围为（0.04～2.0）μmol·L-1,检测限为0.013μmol·L-1。该方法选择性较好、经济简便,能够用于水样中Cr3+的实时检测,检测结果与石墨炉原子吸收光谱法测得的结果吻合。