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771.
用高效毛细管电泳前沿分析法研究了酸性药物那格列奈与人血浆白蛋白的结合常数、结合位点和结合率。使用未涂层的毛细管柱 (4 0cm× 5 0 μmi.d .;有效柱长 32cm) ,磷酸盐缓冲溶液 (pH 7.4 ,离子强度0 .17)为背景溶液 ,在紫外检测波长 2 14nm、运行电压 18kV和重力进样 10 0s的条件下 ,利用那格列奈谱峰的平台高度和游离药物浓度的良好线性关系 (r>0 .999,n =6 ) ,测定了那格列奈的游离药物浓度。固定药物浓度 (2 0 0 μmol L ,2 5 0 μmol L) ,考察不同的蛋白质浓度对结合的影响 ;固定蛋白质浓度 (10 0 μmol L) ,考察不同的药物浓度对结合的影响。实验数据采用非线性拟和程序进行处理 ,得到了那格列奈的蛋白质结合参数。高效毛细管电泳前沿分析法测定的数据重现性良好 (RSD <2 .5 % ,n =3) ,在药代动力学和药效学研究方面具有简便、准确的优点。 相似文献
772.
TA-MS provides chemical and thermal response information. In order for this information to be meaningful sampling must be
performed with minimum dead volume and without cold spots. Dead volume leads to response lag and peak broadening. Cold spots
result in sample condensation, leading to inaccurate data and potentially inlet blockage. This paper describes a hot zone
inlet system and 'in-situ' probe both of which provide fast response, zero dead volume sampling directly to the MS. The paper
also discusses data interpretation methodologies and introduces 'soft ionisation' as a means of providing simplified analysis
of complex mixtures.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
773.
Glassy carbon electrodes modified with (5-amino-1,10-phenanthroline)bis(bipyridine)ruthium(II) chloride hydrate, [(bpy)2Ru(5-phenNH2)]Cl2·H2O, are shown to oxidize hydrazine with excellent sensitivity. The presence of an amine group on the ruthenium complex facilitates electropolymerization onto the electrode surface. Using cyclic voltammetry, a large catalytic current is observed upon oxidation of hydrazine in phosphate buffer (pH 5.0), compared to the current obtained from the ruthenium-modified electrode with no hydrazine present. The sensitivity of cyclic voltammetry is sufficient for obtaining a linear calibration curve for hydrazine over the range of 10−5 to 10−2 M. Hydrodynamic amperometry was used to determine the working potential for flow injection analysis. The limit of detection for hydrazine was determined to be 8.5 μM using FIA. The thickness of these films was shown to increase linearly with the number of electropolymerization cycles, in the range of 1000-2500 nm for 5-20 cycles, respectively, using Rutherford backscattering spectrometry (RBS). RBS analysis also suggests that the film is multilayered with the outermost layers containing a high ruthenium concentration, followed by layers where the concentration of ruthenium decreases linearly and approaches zero at the electrode surface. 相似文献
774.
775.
工业废水中微量铜(Ⅱ)和氰化物的流动注射光度分析 总被引:2,自引:0,他引:2
采用FIA技术,以光度比色法为基础,建立了工业废水中微量Cu^2+和CN^-的顺序自动分析方法和装置。其对二种离子的测定频率为60样/h,相对标准偏差<1.0%,工作曲线的r值≥0.999,各项分析技术指标均优于手工法操作。 相似文献
776.
The molecular structure of Ph3CSSC(S)SCPh3 · CS2 has been determined by X-ray structural analysis. The substance crystallizes in the triclinic crystal system [a = 884.9(2) pm, b = 1 039.5(2) pm, c = 2 064.6(3) pm, α = 75.86(1)°, β = 79.83(2)°, γ = 77.31(5)°, Z = 2, space group P1 ]. The CS3 group is planar; the S? S-bond (201.4 pm) forms an angle of 5.7° with the CS3 plane. The torsional angle CSSC equals 96.3°. (Ph3C)2CS4 was obtained by reaction of TosNSCl2 (Tos = p-MeC6H4SO2) with Ph3CSH in CS2 in the presence of triethylamine. The reaction mechanism is discussed. 相似文献
777.
Ródenas-Torralba E Cava-Montesinos P Morales-Rubio A Cervera ML De La Guardia M 《Analytical and bioanalytical chemistry》2004,379(1):83-89
The aim of this study is to show the advantages of the emerging multicommutation methodology based on the use of solenoid valves for Te determination in milk by hydride generation atomic fluorescence spectrometry (HG-AFS). The delivery of a series of alternating sequential insertions of small volumes of samples and reagents gives rise to new hydrodynamic processes and exciting analytical potentials by controlling the time of flow through the on/off-switched solenoid valves. This drastically reduces the reagent consumption by a factor of 4 and the generation of effluents (590 mL h–1 instead of 750 mL h–1 generated by the continuous-mode measurement) and also provides an improvement in the laboratory productivity by an increase of the sample throughput (85 h–1 compared to 20 h–1 found in the continuous mode). So, multicommutation is an environmentally and economically sustainable alternative to the methodology based on continuous measurements. The multicommutation-based method developed was applied to tellurium determination in commercially available milk samples; a calibration range of 0.0–0.5 ng mL–1 and a detection limit of 0.20 ng L–1 with average relative standard deviation of 2.1% were found. Comparable results were obtained for a series of samples using both continuous and multicommutation HG-AFS modes. 相似文献
778.
Christos Kokkinos Anastasios Economou Ioannis Raptis Constantinos E. Efstathiou Thanasis Speliotis 《Electrochemistry communications》2007,9(12):2795-2800
This work describes a novel type of bismuth electrode for stripping voltammetry based on coating a silicon substrate with a thin bismuth film by means of sputtering. The bismuth-based sensors were characterized by optical methods (scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray diffraction (XRD)) and as well as by linear sweep voltammetry. Subsequently, the electrodes were tested for the detection of low concentrations of trace metals (Cd(II), Pb(II) and Ni(II)) by stripping voltammetry. Well-formed stripping peaks were observed for trace concentrations of the target analytes demonstrating “proof-of-principle” for these sensors. This type of electrochemical device, utilizing thin-film technology for the formation of the bismuth film, holds promise for future applications in trace metal analysis. 相似文献
779.
X射线荧光光谱法在稀土元素分析中的应用 总被引:6,自引:0,他引:6
本文研究了X射线荧光光谱在混合稀土氧化物和高纯稀土氧化物分析中的应用,并探讨了在常量分析中影响分析准确度和精密度的主要因素;样品及标样制备,基体效应校正方法在痕量分析中降低检测限的方法,选择最佳测量条件,降低背景,与分离富集手段相结合,取得满意的结果。 相似文献
780.
M. P. Sánchez Sánchez J. M. Salas Peregrin M. A. Romero Molina 《Monatshefte für Chemie / Chemical Monthly》1987,118(8-9):883-891
Some news thiopyrimidine derivatives and complexes [4-amino-5-nitroso-6-oxo-1,2,3,6-tetrahydro-2-thio-pyrimidine (TANH), its 2-methylthio derivative (MTH), the ammonium salt ofTANH (sTANH) and six new complexes of formulas: Rh(MT)2Cl · 2H2O, Pd(MTH)2Cl2, Pt(MTH)2Cl4, Au(MTH)Cl3 Pd(TANH)2Cl2 and Au(TAN
–)Cl] have been synthesized and characterized by elemental analysis, IR and1H-NMR spectroscopy techniques. The thermal behaviour of all compounds has also been studied.
Rh(III), Pd(II), Pt(IV) und Au(III) Komplexe von 2-Thiopyrimidin Derivaten
Zusammenfassung Es wurden einige neue Thiopyrimidinderivate und deren Komplexe synthetisiert und mittels Elementaranalyse, IR und1H-NMR charakterisiert: 4-Amino-5-nitroso-6-oxo-1,2,3,6-tetrahydro-2-thio-pyrimidin (TANH), dessen 2-Methylthio-Derivat (MTH), das Ammoniumsalz vonTANH (sTANH) und sechs neue Komplexe der Formeln Rh(MT)2Cl · 2H2O, Pd(MTH)2Cl2, Pt(MTH)2Cl4, Au(MTH)Cl3, Pd(TANH)2Cl2 und Au(TAN –)Cl. Das thermische Verhalten der Verbindungen wurde ebenfalls untersucht.相似文献