【作者】 王爱芳；

【导师】 董学芝；

【作者基本信息】 河南大学 ， 分析化学， 2008， 硕士

【摘要】 在抗生素领域内,喹诺酮类是唯一可以与内酰胺类抗生素相媲美的合成抗菌药,其对大多数敏感菌有快速杀灭作用。环丙沙星是第三代喹诺酮类药物在临床医学中最成功地得到广泛应用的抗生素之一,具有广谱、高效、低毒以及口服吸收完全、体内分布广、不易产生抗药性等特点,是目前最佳的抗感染药物之一。本论文建立了三种测定盐酸环丙沙星的新方法,这些方法不仅可以用于评价环丙沙星药物的重要药效指标之一——药物成分的含量,而且对分析食品和环境样品中的环丙沙星药物残留具有参考价值。论文的主要内容如下:一吖啶橙-罗丹明B能量转移荧光猝灭法测定盐酸环丙沙星研究了吖啶橙(AO)与罗丹明B(RB)的共振荧光能量转移作用。研究表明,在λex/λem = 470/576 nm,十二烷基硫酸钠存在下,吖啶橙与罗丹明B能够发生有效共振荧光能量转移。盐酸环丙沙星的加入,使得能量转移体系中罗丹明B的荧光猝灭,以此建立了荧光共振能量转移法测定盐酸环丙沙星的新方法。盐酸环丙沙星含量在0.02-0.44μg/mL范围内,罗丹明B的荧光猝灭程度与盐酸环丙沙星的浓度呈良好的线性关系,回归方程为:△F = 378.0c (μg/mL) + 11.14,相关系数r = 0.9966,最低检出限为0.013μg/mL。此法用于测定盐酸环丙沙星滴眼液的测定,并与国家标准方法高效液相色谱法相比较,结果一致。二刚果红褪色光度法测定盐酸环丙沙星在弱酸性Britton-Robinson缓冲介质中,盐酸环丙沙星与刚果红染料反应,形成离子缔合物,溶液吸光度明显降低,最大褪色波长在496 nm处,据此建立了测定盐酸环丙沙星的褪色光度法。当CPFX浓度在0.8 ~ 8.0 mg/L范围内时,褪色程度△A与CPFX浓度间呈现良好的线性关系,其线性回归方程为:△A=0.03257c(mg/L)-0.0245,相关系数R=0.9980,最低检出限为0.3376 mg/L。此法用于环丙沙星药物的测定,并与国家标准方法高效液相色谱法相比较,结果令人满意。三环丙沙星(CPFX)-锌(Ⅱ)的配合性能及环丙沙星的含量测定本文研究了环丙沙星(CPFX)-锌(Ⅱ)的配合反应,通过摩尔比法求得了配合物的配比为2:1,计算了配合物的离解度和稳定常数。并且研究发现,锌离子与环丙沙星配合后,使体系的紫外吸收有一定程度提高,据此建立了一个新的测定环丙沙星含量的方法。对环丙沙星药物制剂进行测定,结果令人满意。更多还原

【Abstract】 In the antibiotics family, quinolones antibiotics are the only kind synthesis antibacterial drugs which can compare beauty with lactam kind antibiotics. They have the fast sterilization effect for most sensitive bacteria. Ciprofloxacin are widely applied to the clinical medicine as one of the most successful third generation quinolones drugs. Due to many characteristics such as broad spectrum, efficient, low toxicity and complete oral absorption, wide distribution, hard to cause drug-resistance, Ciprofloxacin has been one of the best anti-infective drugs at present.In the present study, three new analytical methods for the determination of ciprofloxacin hydrochloride were developed. These methods are not only used to evalue the effective component which is as one of the most imporment pharmacodynamics indexes, but applicable in the analysis of pharmaceutical residues like antibodies in environment samples as well as in foods. The major results of thepresent study are listed as below:1. A fluorescence quenching method for the determination of ciprofloxacin hydrochloride by fluorescence resonance energy transfer between acridine orange and rhodamine BThe fluorescence resonance energy transfer between acridine orange and rhodamine B has been studied. It was found that the effective energy transfer occurred between acridine orange and rhodamine B in the sodium dodecyl sulfate atλex /λem = 470 / 576 nm and Britton-Robinson buffer(pH = 7.0). The fluorescence intensity of rhodamine B which had increased sharply in the energy transfer system was regularly diminished by ciprofloxacin hydrochloride, and the quenching fluorescence intensity showed a good linear relationship with the concentration of ciprofloxacin hydrochloride in the range of 0.02 to 0.44μg/mL. The equation of linear regression was△F = 378.0c(μg/mL) + 11.14(correlation coefficient r = 0.9966), the detection limit was found to be 0.013μg/mL. The method was applied to the determination of ciprofloxacin in ciprofloxacin hydrochloride eye drops. It was validated applying the standard addition methodology and using HPLC as a reference method.2. Fading spectrophotometric method for determination of Ciprofloxacin Hydrochloride with Congo RedIn weak acidic of Britton-Robinson buffer medium, ciprofloxacin hydrochloride reacts with Congo Red to form an ion-association complex,and the absorption of Congo Red decreases obviously.The maximum fading wavelength at 496nm.Based on this reaction, a new fading spectrophotometric method was developed for determination of ciprofloxacin hydrochloride. The equation of linear regression was△A=0.03257c(mg/L)-0.0245 (correlation coefficient r = 0.9980) in the range of ciprofloxacin hydrochloride concentration in 0.8—8.0mg/L, the detection limit was found to be 0.3376 mg/L.The method was applied to the determination of ciprofloxacin drugs with good results.3. Complexation characteristics of ciprofloxacin with Zn(Ⅱ)and determination of ciprofloxacinThe complexation characteristics of ciprofloxacin(CPFX) with Zn(Ⅱ)has been studied. The complexing ratio of the complex has been determined to be 2:1 using molar ratio method,and the degree of dissociation and stability constant were calculated. Based on this complex reaction, a simple, rapid and sensitive new method for the UV determination of CPFX was proposed and the reaction conditions were investigated in detail. The method was applied to the determination of ciprofloxacin drugs with good results.更多还原