Determination of Trace Titanium by Solid Substrate－Room Temperature Phosphorimetry with 4,5－Dibromophenylfluorone as Luminescent Ligand and Triton X－100 as Sensitizer

A new highly sensitive solid substrate room temperature phosphorimetry for the determination of trace titanium is proposed based on the sensitization of Triton X-100 to the SS-RTP intensity of 4, 5-dibro-mophenylfluorone-titanium complex adsorbed on the filter paper substrate modified by gelatin. When Triton X-100 was added into the luminescence system, the RTP intensity was raised 3 times stronger than that of the system without Triton X-100. The linear dynamic range of the new method is 0. 64 ～ 3.2 fg/spot (0. 4 μL) with a detection limit of 12.8 ag/spot, and the regression equation of the working curve is △Ip = 482. 0 119.5mTi（Ⅳ) (fg/spot), the correlation coefficient r= 0. 9992, n = 6. The phosphorescence lifetime (r= 0. 85 ms) was also determined. The recoveriesCand RSD) for the determinations of titanium in human hair and tea samples were 101.0% (3. 0%) and 99. 97% (4. 2%), respectively.     

导数-固体基质室温燐光法同时测定痕量对位三联苯和间位三联苯

本文提出间三联苯和对三联苯的二阶导数-固体基质室温燐光法(d²SS-RTP)。本法在λ_ax=288nm,用448nm处正峰和460nm处负峰的峰峰高度值定量测定间三联苯,对三联苯不干扰测定.线性范围0.46～46ng.检出限为0.1ng/斑点.对三联苯用526nm处正峰和548nm处负峰的峰峰高度值测定.间三联苯不干扰.线性范围0.46～46ng.检出限0.07ng/斑点.     

滤纸基质室温燐光法测定痕量硫鸟嘌呤的研究

本文对硫鸟嘌呤在不同的固体基质和重原子微扰剂存在下的RTP发射强度进行了比较。结果表明,适宜的固体基质是国产慢速定量滤纸,有效重原子盐为NaI或In_2(SO_4)_3。在此基础上对响影硫鸟嘌呤RTP发射强度的各种因素进行了研究,建立了测定痕量硫鸟嘌呤的SS-RTP法。以NaI为重原子时,方法的线性范围为3.3～200.4ng,检出限为0.4ng/斑点。以In_2(SO_4)_3为重原子时,线性范围为3.3～334.3ng,检出限为1.6ng/斑点。     

同步扫描-固体基质室温燐光法同时测定痕量2,6-二氨基嘌呤和硫鸟嘌呤的研究

本文提出了测定痕量2,6-二氨基嘌呤(DAP)和硫鸟嘌呤(TG)的同步扫描纸基质室温燐光(RTP)法,重原子体系为碘化钾加醋酸钠;激发和发射单色器波长差△λ=110nm;同步特征峰位波长分别为299nm(DAP)和330nm(TG)。     

固体基质室温燐光分析法测定痕量银

基于AgCl·PVA·Ag+ 吸附FIn- 所形成的离子缔合物AgCl·PVA·Ag+ ·FIn- 能在滤纸基质上发射强而稳定的室温光信号的特性 ,建立了以滤纸为基质的固体基质室温光测定痕量银的新方法。该离子缔合物对应于聚乙烯醇 (PVA)存在下Fajans(法扬斯 )法的终点。在一定条件下 ,离子缔合物的光强度与吸附层的Ag+ 含量成正比 ,线性范围为 1.72～ 8.6× 10 - 1 2 g 斑 ,(0 .4 μL 斑 ) ,工作曲线对应的回归方程ΔIp =2 80 .81+35 4 5mAg+ (10 - 1 2 g 斑 ) ,n =6 ,相关系数r =0 .9995。该方法快速、灵敏、准确。用于人发、茶叶中银的测定 ,与AAS法基本相符。     

同步扫描-导数-固体基质室温燐光法同时测定痕量 2,6-二氨基嘌呤和硫鸟嘌呤的研究

本文首次提出以滤纸为基质,以Nal和NaAc为重原子体系,同时测定2,6-二氨基嘌呤和硫鸟嘌呤的同步扫描-一阶导数-SS-RTP分析法。该法简便快速,选择性好,线性范围宽,检出限低。2,6-二氨基嘌呤的线性范围为6～300ng,检出限为0.7ng/斑点;硫鸟嘌呤的线性范围为6.7～167ng,检出限为0.09ng/斑点。     

固体基质室温燐光法中微晶包埋刚性化机理的研究

本文利用扫描电镜对不同的固体基质表面进行了观察。发现它们的表面都存在一个容易使样斑形成微晶微粒的粗糙表面环境。燐光体——硫鸟嘌呤包埋刚性化的实验进一步证实了微晶包埋刚性化也能诱导出强的RTP发射信号。本文提出了另一条新的诱导RTP发射的途径——微晶包埋刚性化机理。     

Strong Luminescence Catalytic Solid Substrate Room Temperature Phosphorescence for the Determination of Trace Copper

Under the conditions of reacting at 100°C for 8 min and irradiating with the infrared light for 15 min, methylene blue (MEB) could emit weak room temperature phosphorescence (RTP) on the cellulose acetate membrane (CAM) using Pb²⁺ as the ion perturber in the NH₃‐NH₄Cl (pH=9.80) solution. MEB was oxidized by H₂O₂, which caused the RTP of the system to enhance. Cu²⁺ could catalyze the reaction of H₂O₂ oxidizing MEB, which caused the RTP of the system to enhance sharply. The ΔI_p (I_p0?I_p, the I_p0 and I_p were RTP intensity of the blank reagent and RTP intensity of the test reagent, respectively) of the catalytic system was 133.6, which was 4.1 times larger than that without infrared light irradiation (33.1). Its ΔI_p was proportional to the content of Cu²⁺. Thus, a new catalytic solid substrate room temperature phosphorimetry (SSRTP) for the determination of trace copper has been established. The limit of quantization (LOQ) of this method was 0.12 ag·spot^?1 (sample volume: 0.40 µL·spot^?1, corresponding concentration: 3.0×10^?16 g·mL^?1), showing high sensitivity. This method not only has been successfully applied to the determination of trace copper in the tobacco, tea and human serum, but also could predict human diseases. The catalytic reaction was first order reaction, whose activation energy (E) was 18.17 kJ·mol^?1 and rate constant (k) was 3.4×10^?4 s^?1. At the same time, the mechanism of catalytic SSRTP for the determination of trace copper was discussed.     

Determination of Trace Mercury by Catalytic Solid Substrate-room Temperature Phosphorimetry

There are some methods for the determination of trace Hg2 such as atomic fluorescence spectrometry (LD: 2.0×10-11 g mL-1)1, catalytic discoloration photometric method (LD: 1.2×10-12 g mL-1)2, bulk optode modified by dithizone (LD: 8.0×10-9 g mL-1)3, c…     

催化K2S2O8氧化靛红固体基质室温磷光法测定痕量Se(V)

基于痕量Se4+催化K₂S₂O₈氧化靛红（Isa）的灵敏反应而导致体系的磷光剧烈猝灭的学术思想,建立了一种高灵敏（检出限（LD）为0.015 pg/mL）催化固体基质室温磷光法(SS RTP)测定痕量Se（IV)的新方法。方法的线性范围为4.00×10–8~4.00×10–6 μg/mL。工作曲线的回归方程为△I_P=2.948+63.24C_Se(IV)(pg/mL),n = 7。相关系数( r )为 0.9997。方法已成功用于水样中痕量Se（IV）的测定,结果与紫外分光光度法相吻合,并探讨了测定痕量Se（IV）的反应机理。     

A New 4.0-Generation Dendrimer Phosphorescence Labeling Reagent and Its Application to Determination of Trace Alkaline Phosphatase by Affinity Adsorption Solid Substrate-room Temperature Phosphorimetry

A Triton X-100-4.0G-D （4.0G-D refers to a 4.0-generation dendrimer） was brought forward as a new phosphorescence labeling reagent. Two types of specific affinity adsorption （AA） reactions （direct method and sandwich method） were carried out between the labeling product of Triton X-100-4：0G-D-Wheat germ agglutinin （WGA） and alkaline phosphatase （ALP）, the product of AA reaction preserved the good characteristics of room temperature phosphorescence （RTP） of 4.0G-D and △Ip of the product was proportional to the content of ALP. According to the fact stated above, a new method for the determination of trace ALP by affinity adsorption solid substrate-room temperature phosphorimetry （AA-SS-RTP） was established on the basis of WGA labeled with the Triton X-100-4.0G-D. The detection limits were 0.20 ag·spot^-1 （corresponding concentration： 5.0×10^-16 g·mL^-1, namely 5.0×10^-18 mol·L^-1） for a direct method and 0.14 ag·spot^-1 （corresponding concentration： 3.5×10^-16 g·mL^-1, namely 3.5×10^-18 mol·L^-1） for a sandwich method, respectively. For their high sensitivity, good repeatability and high accuracy, the direct method and sandwich method have been successfully appfied to determine the content of ALP in human serum, and the results were coincided with the clinical detection results of the enzyme-linked immunosorbent assay method by the Zhangzhou Hospital of Traditional Chinese Medicine. Meanwhile, the mechanism for the determination of trace ALP by AA-SS-RTP was discussed.     

Peroxyoxalate Chemiluminescence Based on Fluorescent Conjugated Polymer for the Determination of Triton X-100

A novel peroxyoxalate chemiluminescence system has been designed for the determination of Triton X‐100 (TX‐100), in which a hydrophobic fluorescent conjugated polymer, poly[2,5‐bisnonyloxy‐1,4‐phenylene‐ethynylene‐9,10‐anthrylene] (PPEA) was employed as a fluorophor. A strong enhanced intensity of chemiluminescence (CL) was observed in the presence of TX‐100, due to the improved emission efficiency of PPEA in the presence of TX‐100. Under optimum conditions, the detection range of Triton X‐100 is between 1.0×10^?7 and 1.0× 10^?4 mol·L^?1, with a detection limit at 6.0×10^?8 mol·L^?1. The relative standard deviation is 2.4% (n=6) for 1.0×10^?6 mol·L^?1 Triton X‐100. This method provides satisfying results in the detection of TX‐100 in nature water and biological samples with high sensitivity and wide linear range.     

以阴离子交换纤维素膜作基质室温燐光法测定痕量2,6-二氨基嘌呤的研究

本文对2,6-二氨基嘌呤(DAP)在不同的基质上和不同的重原子微扰剂存在下的室温燐光(RTP)强度进行比较,结果表明,NaI-NaAc是有效的重原子体系。适宜的固体基质为阴离子交换纤维素(二乙氨基乙基纤维素)膜(DEAE)和慢速定量滤纸。前者对酸度的变化具有较好的缓冲能力,本文提出了以DEAE为固体基质,测定痕量DAP的RTP法。     

同步扫描-微乳状液增稳室温磷光法同时测定痕量多环芳烃的研究

同步扫描－微乳状液增稳室温磷光法同时测定痕量多环芳烃的研究杨欣,董川,魏雁声,晋卫军,刘长松（山西大学化学系,太原,０３０００６）关键词同步扫描－微乳状液增稳室温磷光法;化学除氧技术;多环芳烃１９７８年Ｖｏ－Ｄｉｎｈ等［１］将固定波长同步扫描技术用于...     

亮黄-曲通X-100体系共振瑞利散射法测定蛋白质

基于在TrtionX-100存在下，蛋白质对有机染料亮黄瑞利光散射的增强作用。拟定了测定蛋白质的瑞利光散射光，由于添加了TritonX-100，对不同的蛋白质，测定的灵敏度提高了5－11．8倍，线性范围在0－5．0mg/L之间，最低检测限为10．2μg/L。     

催化过氧化氢氧化邻苯三酚红固体基质室温燐光猝灭法测定痕量钴

基于硼砂缓冲液中聚丙烯酰胺(PAM)存在下,邻苯三酚红(PGR)于滤纸固体基质上能发射强而稳定的室温燐光,PAM可活化钴离子催化H2O2氧化PGR反应,使PGR的室温燐光猝灭,从而建立了测定痕量钴的新方法。该方法的线性范围为4.8~960(×10-18g/斑)Co2+(浓度范围0.012~2.40×10-9g/L,0.4μL/斑),工作曲线的回归方程ΔIp=12.76+0.1248 mCo2+(×10-18g/斑),n=7,相关系数r=0.9993;检出限为1.2×10-18g/斑(对应浓度为3.0×10-12g/L)。对4.8和960(×10-18g/斑)Co2+重复测定11次(0.4μL点样量),RSD分别为3.6%和4.7%。用PAM比不加PAM时ΔIp增加4.6倍。本方法灵敏、准确、简便快速、重现性好,用于党参、当归、川芎、金银花和VB12中的痕量钴测定,结果满意。     

Determination of Glucose by Affinity Adsorption Solid Substrate‐room Temperature Phosphorimetry Based on Triticum Vulgare Lectin Labeled with Silicon Dioxide Nanoparticle Containing Fluorescein Isothiocyanate

In the presence of heavy atom perturber Pb2＋, silicon dioxide nanoparticle containing fluorescein isothiocyanate (FITC-SiO2) could emit a strong and stable room temperature phosphorescence (RTP) signal on the surface of acetyl cellulose membrane (ACM). It was found in the research that a quantitative specific affinity adsorption (AA) reaction between triticum vulgare lectin (WGA) labeled with luminescent nanoparticle and glucose (G) could be carried on the surface of ACM. The product (WGA-G-WGA-FITC-SiO2) of the reaction could emit a stronger RTP signal, and the ΔIp had linear correlation to the content of G. According to the facts above, a new method to determine G by affinity adsorption solid substrate room temperature phosphorimetry (AA-SS-RTP) was established, based on WGA labeled with FITC-SiO2. The detection limit (LD) of this method calculated by 3Sb/k was 0.47 pg•spot－1 (corresponding to a concentration value 1.2×10－9 g•mL－1, namely 5.3×10－9 mol•L－1), the sensitivity was high. Meanwhile, the mechanism for the determination of G by AA-SS-RTP was discussed.     

燐光探针法研究不同变性剂对大肠杆菌碱性磷酸酶构象的影响

通过监测大肠杆菌碱性磷酸酶 (AP)的 10 9位色氨酸 (Trp 10 9)室温光 (RTP)的强度与寿命的变化 ,探讨了变性剂酸、盐酸胍及EDTA对AP构象变化的影响。结果表明 :光强度、光寿命与Trp 10 9所处的微环境刚性化程度有密切的关系。尤其是盐酸胍的加入 ,AP经历了典型的 3种变化状态 :从稳定折叠态到中间态 ,最后形成展开态。极少量的EDTA加入 ,导致蛋白质变性、光减弱和光寿命缩短。     

固体基质室温燐光法测定L-色氨酸

本文提出在Na_2 CO_3存在下,以NaI为重原子微扰剂,以滤纸为基质的L-色氨酸的室温燐光(RTP)测定法。本法不需通干燥气体,工作曲线的线性范围较宽,用于谷物试样分析,得到了满意的结果。