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     

司帕沙星含量的HPLC测定

司帕沙星是一类喹诺柄类抗菌药物,该文采用反相高效液相色谱法对其生产进行质控分析,测定中选用Ｃ１８柱,以甲醇－水（内含４０ｍｍｏｌ．Ｌ＾－１的磷酸二氢钾和３０ｍｍｏｌ．Ｌ＾－１的四乙基溴化铵,Ｖ甲醇：Ｖ水＝４５：５５）为流动相,于２９８ｎｍ进行检测,样品测定的回收率为９７．９％～１００．２％,相对标准偏差不大于２％。     

司帕沙星-亚硝酸荧光体系性质的研究及应用

首次提出了亚硝酸氧化司帕沙星的荧光反应测定司帕沙星的新方法 ,在酸性介质中 ,亚硝酸氧化司帕沙星继而与碘化钾反应生成了新的荧光物质 ,其荧光发射较司帕沙星强 1 3 4倍 ,激发和发射波长分别为 2 86nm和464nm,,当司帕沙星的浓度为 2× 1 0 - 8mo L L～ 1× 1 0 - 6mo L L时 ,工作曲线呈良好的线性关系 ,检出限为 1 .5×1 0 - 1 0 mo L L。据此建立了同步 -导数荧光光谱法测定尿液中司帕沙星的新方法 ,本文还对反应产物的荧光特性及有关反应机理进行了探讨。     

司帕沙星软膏的制备与质量控制

为研制司帕沙星软膏，建立其含量测定方法。用差示紫外分光光度法在306nm外测定司帕沙星的含量。平均回收率为99．98％，RSD为0．72％，线性范围15．62－40．14μg/ml。该法简便、准确、快捷。     

司帕沙星与茜素红荷移反应的研究

采用紫外分光光度法研究了π电子受体茜素红与电子给予体司帕沙星的荷移反应。确定了反应条件,建立了一种快速简便灵敏准确测定司帕沙星的荷移分光光度法。结果表明,司帕沙星与茜素红在(4+6)乙醇-水介质中,室温条件下即可形成1∶1稳定的荷移络合物,该络合物的最大吸收波长为530 nm,表观摩尔吸光系数为4.8×103L.mol-1.cm-1,司帕沙星药物质量浓度在6~160mg/L范围内服从比尔定律,r=0.9991。当该法用于片剂中司帕沙星的测定时,回收率为99.75%~100.00%,相对标准偏差为1.4%(n=10)。     

司帕沙星与卤素反应产物的荧光特性及其应用

研究了卤素（F,Cl,Br,I)与喹诺酮类药物司帕沙星反应产物的荧光特性,发现在酸性介质中,亚硝酸可氧化司帕沙星继而被卤素取代,所得产物具有强烈的荧光发射,其荧光强度随着卤素原子半径的增大呈现规律的增强效应。司帕沙星卤代物荧光较司帕沙星强58－151倍。据此建立了卤素增强荧光光谱测定司帕沙星的新方法。该方法用于直接测定尿液中司帕沙星的含量,结果令人满意。本文还对司帕沙星的荧光增敏机理进行了探讨。     

赖氨酸与邻氯苯甲醛的衍生化反应及其示波极谱法测定

本文研究了赖氨酸与邻氯苯甲醛的衍生化反应,发现所生成的席夫键产物,在约0.30mol/L的磷酸盐缓冲溶液中(pH11.0),于峰电位-1.12V处,在滴汞电极上产生灵敏吸附还原波。导数波高与赖氨酸浓度在1×10~(-7)mol/L～5×10~(-4)mol/L内有线性关系,检测限为3×10~(-8)mol/L。该方法应用于食品中赖氨酸含量测定,得到满意结果。     

司帕沙星的吸附伏安特性及其应用

在0.2mol·L-1 KH2PO4-K2HPO4(pH6.80)底液中,司帕沙星(sparfloxacin,简称SPFX)在汞电极上有一线性扫描还原峰,峰电位Vp= -1.40V(vsAg/AgCl),该峰具有明显的吸附性 ;吸附粒子为SPFX中性分子,测得SPFX在汞电极上的饱和吸附量Гs =5.08×10-11 mol·cm-2,每个SPFX分子所占电极面积为3.27nm2,SPFX在汞电极上的吸附符合Langmuir吸附等温式 ;测得吸附系数 β=1.04×106,25℃时的吸附自由能ΔGФ= -34.33kJ·mol -1,电极反应电子数n=2,不可逆体系动力学参量αnα=1.54,表面电极反应速率常量ks=0.29s -1 ;建立了吸附溶出伏安法测定SPFX的最佳条件,方法的检出限为2.0×10 -8mol·L -1。     

阻抑荧光动力学法测定痕量司帕沙星

研究了Tris水溶液中司帕沙星对Cu（Ⅱ）催化H2O2氧化罗丹明B荧光猝灭体系的抑制作用,发现司帕沙星的质量浓度在0.098～1.372 ng/mL范围内与该体系的荧光强度成良好的线性关系,据此,建立了动力学荧光测定痕量司帕沙星的新方法.该方法检出限可达0.058 ng/mL,并用于制剂及体液中司帕沙星的分析,回收率为98.3%～102.1%.     

线性扫描伏安法研究司帕沙星的电化学行为

采用线性扫描伏安法和循环伏安法研究司帕沙星的电化学行为。在0.05 mol·L~(-1)硫酸溶液中,司帕沙星于-1.29 V(vs.Ag/AgCl)处产生一灵敏的还原峰,司帕沙星的浓度在1.0×10~(-6)～1.5×10~(-4)mol·L~(-1)范围内与其峰电流呈线性关系,检出限(3S/N)为2.0×10~(-7)mol·L~(-1)。该法用于司帕沙星片剂的分析,回收率为96.2%～105.0%,相对标准偏差(n=6)为2.4%。试验证实:司帕沙星在电极上产生的峰为具有吸附性的完全不可逆的还原峰。     

Study on Fluorescence Property of Sparfloxacin Derivatizing System and its Application

Spartloxacin (SPFX) is the fourth generation of the antibacterial quinolones. Due to itsintensive and efficient antibacterial activity compared to the common quinolones '. it hasbeen widely used in clinical practice. Nevertheless. because of the structural dit'ferencesbetween SPFX and other quinolones. the fluorescence of SPFX is so weak that it can notbe determined by means of fluorescence spectra. Hence, it will be of great interest tomake a detailed study on its fluorescence enhancemen…     

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.     

Stability Indicating Hplc Method for the Determination of Sparfloxacin (Spar)

ABSTRACT

A rapid, sensitive and stability indicating method for the determination of sparfloxacin (SPAR) by RP - HPLC has been developed on a Merck RP - Select B (5 μm; 12.5 cm x 4.0 mm) column using a mobile phase of water: acetonitrile: triethylamine (80 : 20 : 0.2 v/v) pH of which was adjusted to 2.6 with orthrophosphoric acid. The flow rate was 1 ml / min. and the detection was carried out at 304 nm using Waters 486 variable wavelength detector. The retention time for SPAR was 7.2 min. Linearity range was from 8 - 1000 ppm. The method showed good precision and accuracy when applied to two brands of tablets containing SPAR. In alkaline media SPAR is stable where as it undergoes degradation in acidic and oxidising conditions generating different degradation products the nature of which is required to be established. The proposed method nicely separates the degraded products from SPAR and hence can be used as stability indicating method for the assay of SPAR.     

紫杉醇及其修饰物的光谱研究

紫杉醇 (paclitaxel,商品名 Taxol)是二萜类化合物 [1] ,对多种肿瘤细胞模型有特殊疗效 .由于它在水中极难溶 (<0 .0 0 4 mg/m L ) ,影响了临床应用 ,有大量关于合成紫杉醇衍生物的研究 ,试图找到增大紫杉醇水溶性的途径 .我们曾用血清白蛋白修饰紫杉醇 ,使其水溶性有一定程度提高 [2 ] .本文对紫杉醇及其修饰产物进行紫外和荧光光谱研究 ,希望找到一种测定紫杉醇修饰的方法 ,并对修饰物的结构进行了讨论 .1　材料和方法1 .1　试剂和仪器　牛血清白蛋白 (Bovine serum albumin,BSA)为电泳纯 ,购自中国医学科学院血液研究所 .紫杉醇购自天…     

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…     

足球分子的电子结构和UV谱的研究

用INDO/2和INDO/CI方法研究了足球分子的电子结构和UV谱。几何构型优化后得到2种键长:R_(5-6)=1.4507,R_(6-6)=1.3979,相应的键序为1.1356和1.4385。SCF计算得到120个成键轨道和120个反键轨道,符合我们建议的结构规则。足球分子的光谱计算结果是振子强度不为零的跃迁只有一个,其值为386.0 nm,和实测的UV谱符合得较好。