测定司帕沙星的化学发光分析方法

基于在氢氧化钠介质中,司帕沙星对luminol-H2O2化学发光体系有明显的抑制作用,结合流动注射分析技术,建立了流动注射化学发光法测定司帕沙星药物的新方法.在优化的实验条件下,测定司帕沙星的线性范围是1.0×10-7-1.0×10-5mol·L-1,检出限为1.0×10-8mol·L-1,相对标准偏差（1.0×10-7mol·L-1的司帕沙星,n=11）为1.4％.     

司帕沙星的单扫示波极谱法

在 0 .2 mol·L- 1KH2 PO4 - K2 HPO4 ( p H6.80 )底液中 ,用单扫示波极谱法可以得到一个灵敏的司帕沙星导数还原峰 ,其峰电位 Ep=- 1 .43V( vs.SCE) ,导数峰电流与司帕沙星浓度在 0 .1～ 8.0μmol· L- 1范围内呈线性关系 ,检出限为 0 .0 5μmol· L- 1。该法应用于模拟尿样和胶囊中司帕沙星质量含量的测定 ,结果满意。对司帕沙星在汞电极上的电化学行为进行了探讨     

Determination of Sparfloxacin in Human Urine by Reversed-Phase High Performance Liquid Chromatography With Nitrous Acid and Hydroiodic Pre-Column Derivatization

Quinolone drugs, due to the aromatic systems with benzoheterocycle in their molecules, can usually emit strong fluorescence. However, contrary to this, sparfloxacin (SPFX) as the fourth generation quinolone products, can only emit weak fluorescence, although it possesses a similar structure to quinolones. At present, the majority of SPFX determinations have been carried out using techniques such as colorimetry1 and spectrophotometry2-3. For the high performance liquid chromatography (HP…     

Studies on Reaction Mechanism Between Sparfloxacin and Bovine Serum Albumin

The binding of sparfloxacin and bovine serum albumin(BSA) in aqueous solution was studied by means of fluorescence and absorbance spectra, and the interactions influenced by Fe^3 and Cu^2 were explored. Based on the Scatchard‘s site binding model and fluorescence quenching, practical formulas for a small molecule ligand attaching to a bio-macromolecule are proposed. The binding parameters were measured according to the suggested models, and the binding distance, the transfer efficiency of energy between sparfloxacin and BSA were obtained in view of the F6rster theory of non-radiation energy transfer. The effect of sparfloxacin on the conformation of BSA was analyzed by means of synchronous fluorescence spectroscopy.     

司帕沙星金属络合物在胶束体系中的荧光特性研究及应用

研究了在金属离子存在下司帕沙星在胶束体系中的荧光特性,首次发现锌（Ⅱ）和阴离子表面活性剂十二烷基硫酸钠对司帕沙星的荧光有显著的协同增敏作用,据引建立了测定人体尿液中司帕沙星含量的同步－导数荧光光谱法,定量线性范围为０．０４～４．０ｍｇ／Ｌ,检测限为０．０４ｍｇ／Ｌ。相对标准偏差为１．６％～３．９％。探讨了锌（Ⅱ）和十二烷基硫酸钠对司帕沙星荧光的增敏机理。     

司帕沙星的毛细管电泳高频电导法测定

采用毛细管电泳高频电导法检测了司帕沙星。探讨了缓冲液的种类、浓度、添加剂以及操作电压和进样时间等因素对分离的影响。选择3.0mmol LHAc-5.0?H5OH(V V)为电泳介质,分离电压20.0kV,在4min内可实现司帕沙星的分离检测。在优化条件下,司帕沙星的线性范围为6 0～280 0μg mL,检出限为1 9μg mL。在该条件下,片剂中的敷料不干扰测定,可成功测定片剂中的司帕沙星,样品回收率为98.7%～101%。     

四溴荧光素荧光猝灭法测定司帕沙星

基于司帕沙星能够猝灭四溴荧光素的荧光且荧光猝灭程度与司帕沙星的量成正比,建立了一种测定微量司帕沙星的方法。在pH3．5的Clark—Lubs缓冲溶液中,四溴荧光素激发波长λex=485nm、发射波长λem=545nm,司帕沙星的质量浓度在0～2．0mg／L范围内符合比耳定律,方法检出限为42．7μg/L。已用于片剂及胶囊中司帕沙星的测定。6次平行测定回收率为93．8％～104．3％,相对标准偏差为1．1％～2．8％。     

Simultaneous determination of methotrexate and metoclopramide in physiological fluids using RP-HPLC with ultra-violet detection; application in evaluation of polymeric nanoparticles

Methotrexate (MTX) is an anticancer drug while metoclopramide (MCP) is an antiemetic agent. Both the drugs are commonly coprescribed to avoid the emesis caused by anticancer drug. In this study, a novel, rapid, sensitive, and cost-effective reverse-phase high-performance liquid chromatography method was developed and validated for simultaneous determination of the methotrexate and metoclopramide in biological and pharmaceutical samples using sparfloxacin as internal standard. The analytes were separated on a Kromasil 100-5C18 RP (250?×?4.6?mm, 5?µm) column, methanol, and 0.05% trifloroacetic acid (36:64?v/v) as mobile phase with a flow rate of 1?mL/min, detection wavelength of 290?nm, and column oven temperature at 40°C. Both the analytes were extracted from physiological fluids (bovine aqueous humor, vitreous humor, and human plasma) using mixture of methanol and 10% perchloric acid (50:50 v/v). The method was linear over the concentration range of 0.025–1.0?µg/mL for methotrexate and 0.030–1.0?µg/mL for metoclopramide. The % recovery from human plasma was 98.57 and 96.74% for MTX and MCP, respectively, while from aqueous humor and vitreous humor was 95.84 and 98.51% for MTX.

The developed method was applied for in vitro release of MTX from polymeric nanoparticles and can be applied for analysis of pharmaceutical and biological samples containing both the drugs.     

Structure,cyclic voltammetry and DNA-binding properties of the bis(pyridine)bis(sparfloxacinato)nickel(II) complex

The neutral mononuclear nickel(II) complex with the quinolone third-generation antibacterial drug sparfloxacin in the presence of the nitrogen-donor heterocyclic ligand pyridine has been synthesized and characterized. Sparfloxacin is deprotonated acting as a bidentate ligand coordinated to the Ni(II) ion through the ketone oxygen and a carboxylato oxygen. The crystal structure of bis(sparfloxacinato)bis(pyridine)nickel(II), 1, has been determined with X-ray crystallography. The cyclic voltammograms of the complex have been recorded in dmso solution and in 1/2 dmso/buffer (containing 150 mM NaCl and 15 mM trisodium citrate at pH 7.0) solution and the corresponding redox potentials have been estimated. The biological activity of the complex has been evaluated by examining its ability to bind to calf-thymus DNA (CT DNA) with UV and fluorescence spectroscopies and cyclic voltammetry. UV study of the DNA-interaction of the complex has shown that it can bind to CT DNA and the DNA-binding constant has also been calculated. The cyclic voltammograms of the complex in the presence of CT DNA have shown that the complex can bind to CT DNA by the intercalative mode. Competitive study with ethidium bromide (EB) has shown that the complex can displace the DNA-bound EB indicating that the complex binds to DNA in strong competition with EB for the intercalative binding site.     

司帕沙星氯代物的制备及荧光性质研究

司帕沙星在酸性介质中与亚硝酸反应 ,其重氮盐在氯化亚铜存在下 ,继而与氢氯酸反应生成一种较司帕沙星荧光响应值高 1 1 0倍的强荧光物质 ,采用元素分析、红外光谱和质谱对其衍生物的结构进行了表征。结果表明 ,司帕沙星的荧光强度与其喹啉环 5 位上的氨基密切相关 ,本文还对司帕沙星的荧光自猝灭及氯代荧光增敏机理进行了探讨。