基于过氧化氢-桑色素化学发光体系的硫化物检测

在pH=9～10范围内,过氧化氢与桑色素溶液混合后可产生较弱的化学发光,表面活性剂十六烷基三甲基溴化铵(CTMAB)和S2-对该体系化学发光有较强的增敏作用,据此建立了H2O2-桑色素-CTMAB化学发光体系测定S2-的新方法,并对该体系的化学发光反应机理进行了研究.在最佳的实验条件下,S2-在(0.9～9.0)×10...     

Synthesis of magnetic nanoparticles for analytical applications

A simple method based on magnetically assisted chemical separation has been developed for analytical purposes. In this method, morin-modified magnetic nanoparticles were used for the selective extraction and preconcentration of copper ions from aqueous solutions. The influence of different parameters, such as the presence of the morin extractant, the amount of morin extractant loaded on the nanoparticles, the pH, adsorption time and the type and minimum amount of eluent required for elution of the copper from the magnetic nanoparticles, were evaluated. The detection limit of the proposed method followed by ICP–OES was found to be 1.3 µg L^?1 and a dynamic linear range of 10–200 µg L^?1 was obtained. The relative standard deviation was less than 5%. The method was applied to the recovery and determination of copper in real samples.     

Fluorescent analysis of interaction of flavonols with hemoglobin and bovine serum albumin

We have studied the fluorescent properties of flavonols (quercetin, fisetin, morin, rutin) with the aim of studying possible interaction with hemoglobin and bovine serum albumin (BSA). We observed an increase in the intensity of intrinsic fluorescence for all the flavonols except rutin in the presence of BSA. From the changes in the fluorescence spectra, we concluded that tautomeric forms are formed on interaction with hemoglobin. We determined the interconnection between the structure of related flavonols and their fluorescent properties on interaction with proteins, and we determined the binding constants for binding with BSA and hemoglobin. __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 74, No. 5, pp. 659–664, September–October, 2007.     

Adsorptive stripping voltammetric determination of antimony

A new method is described for the determination of antimony based on the cathodic adsorptive stripping of Sb(III) complexed with 2′,3,4′,5,7-pentahydroxyflavone(morin) at a static mercury drop electrode (SMDE). The reduction current of the adsorbed antimony complex was measured by 1.5th-order derivative linear-sweep adsorption voltammetry. The peak potential is at −0.51 V (vs. SCE). The effects of various parameters on the response are discussed. The optimized analytical conditions were found to be: supporting electrolyte, chloroacetic acid (0.04 mol/l, pH 2.3); concentration of morin, 5×10⁻⁶ mol/l; accumulation potential, −0.25 V (vs. SCE); scan rate, 100 mV/s. The limit of detection and the linear range were 7×10⁻¹⁰ mol/l and 1.0×10⁻⁹3.0×10⁻⁷ mol/l Sb(III) for a 2-min accumulation time, respectively. This method has been applied to the determination of Sb(III) in steel and brass samples and satisfactory results were obtained. The adsorptive voltammetric characteristics and composition of the Sb(III)–morin complex were studied.     

桑色素金属(Ⅱ)固体配合物的抗氧性研究（英文）

本文报道了五种金属(Ⅱ)桑色素固体配合物的合成.通过元素分析、溶解尔电导、红外光谱、热重差热、核磁共振氢谱和荧光分析测定了配合物的组成和性质，结果表明配合物组成为ML2*nH2O[M=Mn(Ⅱ)、Co(Ⅱ)、Ni(Ⅱ)、Cu（Ⅱ)、Zn(Ⅱ)；L=Morin(失去2`-OH中质子）；n=2或3].并对配体、配合物进行了脂质过氧化物生成的抑制和清除O-2。自由基的对比研究。     

聚乙烯吡咯烷酮增敏荧光光度法测定生物样品中痕量铅

研究了聚乙烯吡咯烷酮对桑色素和铅（Ⅱ）络合反应的增敏作用，发现ＰＨ３．４３时Ｐｂ－ｍｏｒｉｎ－ＰＶＰ三元体系在４３５ｎｍ激发下，４４４ｎｍ处有强荧光发射，提出了荧光光度法测定痕量Ｐｂ的新方法，其线性范围为０－２４０μｇ／Ｌ，对空白１１次测定ＲＳＤ为３．５％，检出限为２．１＊１０＾－２ｍｇ／Ｌ。     

Studies on Simultaneous Fluorescence-Spectrophotometric Determination of Ultratrace Niobium(V), Tantalum(V), and Zirconium(IV) Using Partial Least-Squares Algorithm

In the presence of cetyltrimethylammonium bromide, a cationic surfactant, highly sensitive molecular fluorescence reactions occur between Nb(V), Ta(V), and Zr(IV) ions and morin (3, 5, 7, 2′, 4′-pentahydroxyflavone) in acidic medium to form stable ternary micellar complexes. Their λ_ex(max)/λ_em(max)values are 421.0/492.2, 416.2/489.6, and 424.2/507.8 nm, respectively, and their λ_em(max)values are 490.5, 488.6, and 507.2 nm, respectively, at the same fixed λ_exof 420.5 nm, indicating their seriously overlapping fluorescence excitation spectra and fluorescence emission spectra. The linear ranges of their regression calibration curves are 0 to 0.20, 0 to 0.50, and 0 to 0.20 mg/liter, respectively, with 0.5 ng/ml for all of sensitivities. The simultaneous molecular fluorescence-spectrophotometric determination of ultratrace or trace Nb(V), Ta(V), and Zr(IV) without separation was made using a partial least-squares (PLS) algorithm and other algorithms. The optimum PLS computation conditions are wavelength point number of 25 and corresponding wavelength range from 450 to 550 nm oriented from λ_em500 nm to two sides at combined intervals of 2.5 and 5.0 nm at a fixed λ_exof 420.5 nm with an optimum calibration sample number of 14 and respective optimum abstracted factor numbers of 6, 4, and 3. With respect to both accuracy and precision of the obtained results, the PLS algorithm is superior to the ordinary least-squares algorithm.     

桑色素与牛血红蛋白相互作用的光谱研究

利用紫外可见吸收光谱和荧光光谱研究了在生理pH条件下桑色素与牛血红蛋白(BHb)的相互作用。实验结果表明:桑色素分子与BHb发生反应生成基态复合物,导致BHb内源荧光的猝灭,该猝灭属于静态猝灭。测定了不同温度下该反应的表观结合常数、结合位点数及结合热力学参数,热力学参数的变化表明上述作用过程是一个熵增加、自由能降低的自发分子间作用过程,桑色素与BHb之间以疏水和静电作用力为主;根据F-rster能量转移理论,测得供体与受体间结合距离r和能量转移效率E;并用同步荧光光谱法探讨了桑色素对BHb构象的影响。     

Separation of zinc from aqueous samples using a molecular imprinting technique

In this article, the separation of zinc from aqueous samples by solid-phase extraction based on a molecular imprinting technique is described. Zn-imprinted polymer was prepared by free radical solution polymerisation in a glass tube containing ZnSO₄, morin, 4-vinylpyridine as a functional monomer, ethyleneglycoldimethacrylate as a cross-linking monomer, and 2,2′-azobisisobutyronitrile as an initiator. The obtained polymer block was ground and sieved (55–75 µm) and the Zn–morin complex was separated from polymer particles by leaching with 2M HCl. The synthesised polymer particles have been characterised by IR and differential scanning calorimetric studies either before or after leaching. The effects of different parameters, such as pH, adsorption and desorption time, type and minimum amount of the eluent for elution of the complex from polymer were evaluated. Extraction efficiency more than 99% was obtained by elution of the polymers with 10 mL of CH₂Cl₂–dimethyl sulfoxide (1 : 1, v/v). The detection limit of the proposed method was 2.9 µg L^?1. A dynamic linear range in the range of 25–200 µg L^?1 was obtained. The relative standard deviation was found to be below 9.2%. In addition, the influence of various cationic and anionic interferences on the complex recovery was studied. The method was applied to the recovery and determination of Zn in a few different real samples.     

A UPLC–MS/MS method for comparative pharmacokinetics study of morusin and morin in normal and diabetic rats

The aim of this study was to establish and validate a rapid, selective and reliable ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) for simultaneous quantitations of morin and morusin, and to investigate their pharmacokinetics difference between normal and diabetic rats after oral administration. Plasma samples were pretreated via protein precipitation with acetonitrile. Genkwanin was used as internal standard (IS). Analytes and IS were separated on a Thermo Hypersil Gold C₁₈ column (50 × 4.6 mm, 3 μm) using gradient elution. The mobile phase consisted of acetonitrile and 0.1% formic acid in water at a flow rate of 0.5 mL/min. Mass spectrometry detection was carried out by means of negative electrospray ionization source and multipe‐reaction monitoring mode. The transitions of m/z 300.9 → 151.2 for morin, m/z 419.2 → 297.1 for morusin and m/z 283.1 → 268.2 for IS were chosen for quantification. Calibration curves were linear in the range of 1.01–504.2 ng/mL (r² ≥ 0.99) for morin and 1.02–522.3 ng/mL (r² ≥ 0.99) for morusin. The lower limit of quantification was 1.02 ng/mL for morin and 1.05 ng/mL for morusin. The extraction recovery was >85.1% for each analyte. No obvious matrix effect was observed under the present UPLC–MS/MS conditions during all of the bioanalysis. The stability study demonstrated that morin and morusin remained stable during the whole analytical procedure. The method was successfully applied to support the pharmacokinetic comparisons of morin and morusin between normal and diabetic rats.