【作者】 王娟；

【导师】 孙汉文；

【作者基本信息】 河北大学 ， 分析化学， 2012， 硕士

【摘要】 流动注射分析（flowinjectionanalysis，FIA）是一门较年轻的分析技术，具有仪器结构简单、操作简便、易于自动连续分析及速度快、精度高、消耗低、适应性较广等优点，它可与多种分析技术相结合，有力的推动了仪器分析的发展，成为一门新型微量、高速的分析技术。化学发光分析法具有灵敏度高、线性范围宽等特点，已广泛地应用于环境化学、临床检验、药物分析和工业分析等领域。本文结合了上述两种技术，将过渡金属超常氧化态应用于化学发光，建立了检测药物、体液及血液中某些抗生素类药物含量的流动注射化学发光新方法。主要研究内容如下：1.研究了流动注射化学发光检测氧氟沙星及左氧氟沙星含量的新方法，并对二（氢过碘酸）合铜（III）配离子-硫酸-亚硫酸钠化学发光体系的机理进行了探讨。在较广泛范围内，化学发光（CL）强度与药物的浓度呈良好线性关系，其相关系数高于0.9988，氧氟沙星与左氧氟沙星检出限分别为8.7×10^-9g/mL及9.2×10^-9g/mL。片剂、注射液、尿样中氧氟沙星及左氧氟沙星的回收率为88.0¹02.0%，相对标准偏差为1.1².3%，结果使人满意。2.在酸性条件下，头孢米诺钠对铜（III）配合物-硫酸-罗丹明6G化学发光体系有着强烈增敏效应，据此建立了流动注射化学发光法定量分析头孢米诺钠的新方法。方法的线性范围为2.0×10^-7g/mL⁶.0×10^-6g/mL，检出限为1.4×10^-7g/mL。对2.0×10^-7g/mL头孢米诺钠水溶液进行分析，11次平行测定的相对标准偏差为1.69%。利用此方法测定鸡血样和头孢米诺钠针剂中头孢米诺钠的含量，结果满意。3.基于[Cu（HIO₆）₂]5-Cu（III）配合物和鲁米诺在碱性溶液中的反应，本研究提出了测定头孢唑林钠的新方法，对头孢唑林钠增敏[Cu（HIO₆）₂]⁵-luminol化学发光进行了机理探讨。Cu（III）配合物-鲁米诺在碱性、酸性介质中的化学发光有很大不同。考察了反应条件对化学发光的影响。在最佳条件下，化学发光强度与头孢唑林钠在2.0×10^-8g/mL².0×10^-6g/mL浓度范围内有良好的线性关系，相关系数R₂为0.9978，检出限4.6×10^-8g/mL。此方法已用于检测针剂及人体尿样中头孢唑林钠的含量，回收率82.0¹09.0%，RSD0.7².1%，结果令人满意。更多还原

【Abstract】 Flow injection analysis （FIA） is a youthful analysis technology, and it has advantages ofsimple equipment, convenient operation, rapid analysis, high precision, low consumption,安and abroad adaptability. FIA can combine with other analysis technology and this pushesforward development of analysis instrument. It becomes a new type technology of traceanalysis with high speed. Chemiluminescence has feature of high sensitivity and broad linearrange. It was applied to environment analysis, clinical test, pharmaceuticals analysis andindustry analysis abroadly. In this text, applying Cu（III） complex to chemiluminescence,several new methods of FIA-CL were developed for the determination of some antibioticpharmaceuticals in pharmaceuticals, body fluid, and blood by combined the two technologies.The main research content as follow:1. A new flow injection chemiluminescence detection of ofloxacin and levofloxacincontent was established, while the Bis （hydrogen iodate） of Cu （III） complex ion-sulfuricacid-sodium sulfite chemiluminescence system mechanism was investigated. Within thebroader context, the chemiluminescence （CL） intensity and concentration of the drug showeda good linear relationship, with the correlation coefficient of0.9988, ofloxacin andlevofloxacin detection limits respectively were8.7×10^-9g/mL and9.2×10^-9g/mL. Tablets,injection, in urine ofloxacin and levofloxacin, the recovery was88.0to102.0%, relativestandard deviation ranged from1.1to2.3%, the result is satisfactory.2. Cefminox sodium in acidic conditions has a strong sensitizing effect to copper （III）complex-sulfuric acid-rhodamine6G chemiluminescence system, thereby the establishmentof a new method of flow injection chemiluminescence for quantitative analysis of cefminoxsodium. The linear range was2.0×10^-7g/mL⁶.0×10^-6g/mL with the detection limit of1.4×10^-7g/mL. The relative standard deviation was1.69%for11determinations of2.0×10^-7g/mLcefminox sodium. This method was used for the determination of cefminox sodium in theinjection and chicken blood with satisfactory result.3. A novel chemiluminescence （CL） method was developed for the determination ofcefazolin sodium based on the CL reaction between [Cu（HIO₆）₂]5-（Cu（III） complex） andluminol in alkaline solution. CL emission of Cu（III） complex-luminol in alkaline medium wasvery different from that in acidic medium. A possible mechanism of the enhanced effect of cefazolin on CL emission of the [Cu（HIO₆）₂]5--luminol system was proposed. The effect ofthe reaction conditions on CL emission was examined. Under the optimized conditions, agood linear relationship was obtained between the CL intensity and the concentrations ofcefazolin sodium in the range from2.0×10^-8to2.0×10^-6g/mL with correlation coefficent ofR₂=0.9978. The limit of detection was4.6×10-9g/mL. The proposed method was applied forthe determination of cefazolin sodium in real samples with the recoveries of82.0¹09.0%with the RSD of0.7².1%. The proposed method has been successfully applied for thedetermination of cefazolin sodium in injectable powder preparations and human urine withsatisfactory results.更多还原