5,10,15,20—四（3—溴—4—磺酸苯基）卟啉光度法测定痕量铜的研究

本文研究了新水溶剂卟啉试剂５，１０，１５，２０－四（３－溴－４－磺酸苯基）卟啉（Ｔ（３－ＢｒＰ）ＰＳ４）与铜的显色反应，在ｐＨ３，铜与５，１０，１５，２０－四（３－溴－４－磺酸苯基）卟啉形成１：１的稳定配合物，此配合物的最大吸收波长位于４１２．８ｎｍ摩尔吸光系数为２．６１×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１。铜量在０～３．０μｇ／２５ｍＬ范围内符合比尔定律，工作曲线回归方程为ｙ＝ ０．００９４３     

四（4—甲氧基—3—磺酸苯基）卟啉分光光度法测定微量铅

研究了水溶性卟啉５，１０，１５，２０－四（４－甲氧基－３－磺酸苯基）卟啉（Ｔ（４－ＭＯＰ）ＰＳ４）与铅的显色反应，在ｐＨ１１和酒石酸钾存在下铅与Ｔ（４－ＭＯＰ）ＰＳ４在室温时间形成１：１的配合物，其最大吸收波长在位于４６４．４ｎｍ，摩尔吸光系数为２．３×１０＾５Ｌ．ｍｏｌ＾－１．ｃｍ＾－１，铅量在０～２０μｇ／２５ｍＬ，范围为符合比尔定律，工作工线回归方程Ａ＝０．０２６２＋０．０４３５ｃ相关系数ｒ     

（TPPS4）2二聚体系吸光光度法测定铜的研究

研究了ｐＨ４．０－６．０，乙酸－乙酸钠体系中ｍｅｓｏ－四（４－磺酸苯基）卟啉发二聚反应的条件。ＴＰＰＳ４二聚物在４８９ｎｍ处有一个较强的吸收峰，利用Ｖｕ＾２＋－ＴＰＰＳ４络合物的形成使此峰线性降低，从而测定痕量铜，表观摩尔吸光系数为５．０＊１０＾５，与ＡＡＳ值相比较，结果令人满意。     

5,10,15,20—四（3—溴—4—磺酸苯基）卟啉高效液相色谱法测定河水中微量…

研究了新合成的显色剂５，１０，１５，２０－四（３－溴－４－磺酸苯基）卟啉与Ｃｏ（Ⅱ）、Ｚｎ（Ⅱ）、Ｃｕ（Ⅱ）形成配合物离子的反应，在ＺＯＲＢＡＸ ＯＤＳ柱上，用含２０ｍｍｏｌ／Ｌ乙酸－乙酸钠（ｐＨ６．０）和１０ｍｍｏｌ／Ｌ四乙基碘化铵的乙腈－水（２７：７３，Ｖ／Ｖ）流动相洗脱，在４２０ｎｍ波长下检测。Ｃｏ（Ⅱ）、Ｚｎ（Ⅱ）、Ｃｕ（Ⅱ）螯合物在９ｍｉｎ内获得完全分离，检测限分别为０．２ｎｇ，０．０５     

（R）—四氢噻唑—2—硫酮—4—羧酸的合成及其晶体结构

由Ｌ－半胱氨酸盐酸盐与二硫化碳在ＮａＯＨ及ＣｕＳＯ４．Ｈ２Ｏ存在下反应得到（Ｒ）－四氢噻唑－２－硫酮－４－羧酸，「α」＾２０Ｄ－８７．５°，产率６６％。用Ｘ射线衍射法测得其晶体结构，属正交晶系，Ｐｚ１ｚ１ｚ１空间群，晶体学参数：α＝０．５０２９（２）ｎｍ，ｂ＝０．７７４９９（５）ｎｍ，ｃ＝１．６３００（５）ｎｍ，Ｖ＝０．６３５０（５）ｎｍ＾３，Ｚ＝４。用分子轨道方法研究了该化合物的电子结构，得到其     

meso—四（3—氟—4—磺基苯）卟啉与钯（Ⅱ）显色反应的分光光度研究

本文对新多卤代水溶性ｍｅｓｏ－四（３－氟－４－磺基苯）卟啉与Ｐｄ（Ⅱ）的显色反应进行了研究，在ＰＨ４．８，有抗坏血酸存在，沸水浴中加热，形成稳定的１：１配合物，最大吸收波长在４０９ｎｍ处。工作曲线回归方程Ａ＝０．００１＋０．０６４ｘ，相关系ｒ＝０．９９６４。     

锰（Ⅲ）—四（4—氨基苯基）卟啉与单链脱氧核糖核酸间染色反应的研究

本文研究了固定于硝酸纤维素滤膜（ＮＣ）上单链脱氧核糖核酸（ｓｓＤＮＡ）与锰（Ⅲ）－ｍｅｓｏ－四（４－氨基苯基）卟啉（ＭＮ－ＴＡＰＰ）间的染色反应机理及实用性，室温下，在２５～１００ｍｍｏｌ／Ｌ的磷酸缓冲液（ｐＨ５．５～７．０）中，６０～８０μｇ／ｍＬ锰（Ⅲ）－ｍｅｓｏ－四（４－氨基苯基）卟啉可将固定于ＮＣ膜上的ｓｓＤＮＡ染成绿色，低至１０ｐｇ／ｄｏｔ的ｓｓＤＮＡ亦可被检出。     

1,3,3a,5—四苯基—3a,4,5,11—四氢—3H,6H—1,2,4—三唑并（ …

通过２，４－二苯基－２，３－二氢－１Ｈ－１，５－苯并二氮杂Ｚｕｏ与苯甲酰氯苯腙的（２＋３）环加成反应制备了标题化合物，用Ｘ射线单晶衍射仪测定了其晶体结构，晶体属正交晶系，空间群为Ｆｄｄ２．晶胞参数；ａ＝１．７６２８（４）ｎｍ，ｂ＝５．７５１２（１２）ｎｍ，ｃ＝１．０２２７ｎｍ，Ｖ＝１０．３６８（５）ｎｍ＾３，Ｚ＝１６，Ｄｃ＝１．２６２ｇ．ｃｍ＾－３，μ＝０．０７５ｍｍ＾－１，Ｆ（０００）＝４１６０     

脱氧核糖核酸（DNA）的极谱伏安行为研究

研究了脱氧核糖核酸的极谱伏安行为，在０．１ｍｏｌ．Ｌ＾－１ＮＨ４Ｃｌ溶液中ＤＮＡ产生一良好的极谱峰，峰电位Ｅｐ＝－１．６５Ｖ（ｖｓ．Ａｇ／ＡｇＣｌ），且峰电流ｉｐ与ＤＮＡ的浓度在４．５＊１０＾－５－３．７＊１０＾－４ｍｏｌ．ＬＯ＾－１范围内呈线性关系，可望用于ＤＮＡ的定量分析。     

meso—四（4—溴苯基）卟啉与Ag（I）的显色反应光度法研究

研究了ｐＨ１０．０，Ｔｗｅｅｎ－８０存在时，ｍｅｓｏ－四（４－溴苯基）卟啉与Ａｇ（Ｉ）络合显色的反应条件，络合物的最大吸收波长为４２７ｎｍ，表观摩尔吸光系数为３．５×１０５，Ａｇ（Ｉ）在０～０．４８ｍｇ／Ｌ范围内呈线性关系，回归方程为：Ａ＝０．１３１Ｃ＋０．００１２，相关系数γ＝０．９９９８。此法用于纯铅样和照相废液中痕量银的测定，结果与ＡＡＳ结果相比令人满意     

十六烷基溴化吡啶与脱氧核糖核酸作用的共振光散射光谱及其分析应用

在碱性条件下，十六烷基溴化吡啶(CPB)与脱氧核糖核酸(DNA)共存时，体系产生较强的共振光散射，其强度与DNA浓度呈线性关系，据此提出了基于阳离子表面活性剂的共振光散射法定量测定DNA。在最佳实验条件下，测得小牛胸腺DNA(ctDNA)和鱼精子DNA(fsDNA)的线性范围分别为0．2-2．0mg／L和0．2—1．25mg／L，检出限分别为0．07mg／L和0．05mg／L。该方法已应用于合成样品及实际样品中DNA含量的测定。     

Spectrophotometric Studies on the Proton Transfer from the Protonated DNA to 5,10,15,20-Tetrakis[4-(trimethyammonio)-phenyl]porphine

Abstract

The interaction of nucleic acids with 5, 10, 15, 20-tetrakis[4-trimethy-ammonio)phenyl]porpine (TAPP) were investigated on the basis of a mechanistic discussion, and a spectrophotometric method for DNAs was accordingly proposed in the present paper. Depending on the acidity of the solution, TAPP can interact with nucleic acids, producing different absorption features. When the pH of the solution is higher than 6.39, TAPP can interact with both DNAs and RNA, giving a new absorption band at 420.3 nm. If the pH is lower than 6.39, however, the interactions with DNAs (but not RNA) can give an absorption band centered at 436.3 nm. It was found that the absorption band at 436.3 nm originates from the proton transfer from the protonated double-stranded structure of DNA to TAPP. At optimal conditions, the absorbance at 436.3 nm is in proportion to the concentration of the DNAs. Calibration curves were linear in the range of 0±3.0 μg.ml^?1 for calf thymus and 0±3.2 μg.ml^?1 for fish sperm DNA. No interference of 4-fold of RNA was found for the determination of DNAs. The limits of determination (3[sgrave]) were 34.6 ng.ml^?1 for calf thymus DNA and 33.2 ng.ml^?1 for fish sperm DNA, respectively. Four synthetic samples were determined with satisfaction.     

十六烷基三甲基溴化铵增敏砂罗铬花青R共振光散射法检测DNA

在pH=3．92的三羟甲基氨基甲烷-HCl缓冲溶液中,阳离子表面活性剂十六烷基三甲基溴化铵对砂罗铬花青R与脱氧核糖核酸(DNA)的共振光散射(RLS)有协同增强作用。考察了影响因素,研究了在优化条件下RLS强度与DNA浓度之间的关系,鱼精DNA和小牛胸腺DNA的线性范围均为0．05—3．00mg／L,检出限分别31．03、35．98μg/L,回收率为97．9％～99．6％,测定结果的相对标准偏差为0．5％-2．1％。     

Fluorescent Complexes of Nucleic Acids/8-Hydroxyquinoline/Lanthanum(III) and the Fluorometry of Nucleic Acids

Abstract

The ternary fluorescent complexes of nucleic acids/8-hydroxyquinoline/ lanthanum (III) were studied. Nucleic acids in the study involve natured and thermally denatured calf thymus DNA, fish sperm DNA and yeast RNA. In the range of pH 8.0–8.4 (controlled by NH₃-NH₄Cl buffer) ternary fluorescent complexes are formed which emit at 485.0 nm for calf thymus DNA and at 480.0 nm for yeast RNA (when excited at 267.0 nm) and emits at 483.0 nm for fish sperm DNA when excited at 265.0 nm. Based on the fluorescence reactions sensitive fluorometric methods for nucleic acids were proposed. Using optimal conditions, the calibration curves were linear in the range of 0.4–3.6 μg˙ml^?1 for calf thymus DNA, 0.4–4.0 μg-ml^?1 for fish sperm DNA and 0.4–4.0 μg˙ml^?1 for yeast RNA, respectively. The limits of determination (3σ) were 0.076 μg˙ml^?1 for calf thymus DNA, 0.068 μg˙ml^?1 for fish sperm DNA and 0.329 μg˙ml^?1 for yeast RNA, respectively. Five synthetic samples were determined with satisfaction.

     

Determination of DNA with cetyltrimethylammonium bromide by the measurement of Resonance Light Scattering.

A simple assay of DNA was developed based on the measurements of enhanced signals of Resonance Light Scattering (RLS) of cetyltrimethylammonium bromide (CTMAB) by DNA. The enhanced RLS signals, measured by simultaneously scanning the excitation and emission monochromators of a common spectrofluorometer with lambda ex = lambda em, was optimized for the DNA assay with CTMAB. On the conditions of pH 2.21 and ionic strength 0.002, the enhanced RLS intensity at 470.0 nm, delta I, was found to be proportional to the concentration of DNA in the range 0-2.5 micrograms/ml if 1.5 x 10(-5) M CTMAB was used. Limits of determination for calf thymus DNA and fish sperm DNA were 4.9 ng/ml and 9.2 ng/ml, respectively. Synthetic samples were determined with the recovery ratio ranging from 93.2% to 105.1%, and the RSD is lower than 2.7%.     

Application of functionalized CdS nanoparticles as fluorescence probe in the determination of nucleic acids

Nanometer-sized fluorescent particles were successfully synthesized. The nanoparticles have a narrow, tunable, symmetric emission spectrum and a broad, continuous excitation spectrum. They are also photochemically stable. A synchronous fluorescence method was developed for the rapid determination of DNA with functionalized CdS as a fluorescence probe, based on the synchronous fluorescence quenching of functionalized CdS in the presence of DNA. Maximum fluorescence is produced at pH 7.0, with maximum excitation and emission wavelengths of 360 and 620 nm, respectively. The maximum emission wavelength of synchronous fluorescence is 354 nm when delta lambda = 260 nm. Under optimum conditions, the calibration graphs are linear over the range 0-3.5 microg mL(-1) for calf thymus DNA (CT-DNA) and 0.2-3.0 microg mL(-1) for fish sperm DNA. The corresponding detection limit is 0.01 microg mL(-1) for CT-DNA and 0.02 microg mL(-1) for fish sperm DNA. The relative standard deviation of seven replicate measurements is 2.2% for 1 microg mL(-1) calf thymus DNA and 2.4% for 1 microg mL(-1) fish sperm DNA. The method is simple, rapid and sensitive. The recovery and relative standard deviation are very satisfactory.     

Study of the interaction of Azur B with DNA and the determination of DNA based on resonance light scattering measurements

Based on the measurements of molecular absorption and resonance light scattering (RLS), the aggregation of Azur B (AB) was in a medium of pH ranging from 1.98 to 2.56 and ionic strength <0.12 M. The presence of double stranded DNA prompts the aggregation, resulting in enhanced RLS signals. Linear relationships were achieved between the enhanced RLS intensity at 359.7 nm and DNA concentration in the range of 0-4.5 μg ml⁻¹ for both calf thymus DNA (ctDNA) and fish sperm DNA (fsDNA) if 3.0×10⁻⁵ M AB was employed. The 3σ limits of detection were 9.3 and 8.9 ng ml⁻¹ for ctDNA and fsDNA, respectively. Five synthetic samples were analysed satisfactorily.     

用结晶紫测定DNA 的分光光度法

研究了结晶紫与ＤＮＡ的可见吸收光谱和提出了测定ＤＮＡ的分光光度法。在ｐＨ９．５６的条件下,加入ＤＮＡ后结晶紫在５８９ｎｍ的最大吸收峰强度显著下降,下降程度与ＤＮＡ的含量呈线性关系,确定了实验的最佳条件,ＤＮＡ线性响应范围为０～５ｍｇ／Ｌ,检出限１９．５μｇ／Ｌ。该法简便,快速,具有较高的选择性,对合成样品中ＤＮＡ的测定结果令人满意。     

Preparation and application of cysteine-capped ZnS nanoparticles as fluorescence probe in the determination of nucleic acids

Cysteine-capped ZnS nanometer-sized fluorescent particles were produced by a colloidal aqueous synthesis. The functionalized nanoparticles are water-soluble and suitable for biological application. A synchronous fluorescence method has been developed for the rapid determination of DNA with functionalized nano-ZnS as a fluorescence probe, based on the synchronous fluorescence enhancement of cysteine-capped nano-ZnS in the presence of DNA. When Deltalambda =190 nm, maximum synchronous fluorescence is produced at 267 nm at pH 5.12. Under optimum conditions, the synchronous fluorescence intensity is proportional to the concentration of nucleic acids in the range 0.1-1.2 microg ml(-1) for calf thymus DNA, 0.1-0.6 microg ml(-1) for fish sperm DNA. The corresponding detection limit is 32.9 ng ml(-1) for calf thymus DNA and 24.6 ng ml(-1) for fish sperm DNA. This method is simple, inexpensive, rapid and sensitive. The recovery and relative standard deviation are satisfactory.     

Determination of nucleic acids using calcein-neodymium complex as a fluorescence probe.

A novel fluorometric method has been developed for rapid determination of DNA and RNA with calcein-neodymium complex as a fluorescence probe. The method is based on the fluorescence enhancement of calcein-Nd(III) complex in the presence of DNA or RNA, with maximum excitation and emission wavelength at 489 nm and 514 nm, respectively. Under optimal conditions, the calibration graphs are linear over the range 0.5 - 3.0 microg/ml for both DNA and yeast RNA, 0.4 - 2.0 microg/ml for fish sperm DNA (FS DNA) and 0 - 3.0 microg/ml for calf thymus DNA (CT DNA). The corresponding detection limits are 15.1 ng/ml for DNA, 21.2 ng/ml for yeast RNA, 10.5 ng/ml for FS DNA and 8.9 ng/ml for CT DNA. The interaction mechanism for the binding of calcein-Nd(III) complex to DNA is also studied. The results of absorption spectra, fluorescence polarization measurements and thermal denaturation experiments, suggested that the interaction between calcein-Nd(III) complex and DNA is an electrostatic interaction.