几种氟喹诺酮类药物残留和亚硝酸根的检测新方法研究与应用

发布时间：2018-06-06 16:44

  本文选题：诺氟沙星 + 洛美沙星　； 参考：《南华大学》2012年硕士论文

【摘要】：第一章分别介绍了氟喹诺酮类药物诺氟沙星、洛美沙星和环境中污染物亚硝酸根的卫生检验研究意义和当前研究进展，并分别简要阐述了本课题所建立的诺氟沙星、洛美沙星和亚硝酸根三种物质卫生检验新方法的基本原理和定量测定的依据。 第二章为同时测定2种氟喹诺酮类抗生素的含量，研究了诺氟沙星(NFLX)和洛美沙星(LFLX)的同步荧光光谱及其一阶导数同步荧光光谱，利用零交点法避免了它们之间的干扰。在pH=4.0的HAc-NaAc缓冲溶液中， λ=160nm的条件下，测定了诺氟沙星和洛美沙星的同步荧光光谱。进一步对2种沙星的同步荧光光谱做一阶导数处理，分别在NFLX和LFLX的导数同步荧光光谱为零的275.0nm和283.8nm处读取另一种沙星的信号值。该值与浓度呈线性关系，，NFLX和LFLX的线性范围分别为1.68×10~(-8)~5.64×10~(-6)mol·L~(-1)，1.89×10~(-8)~6.19×10~(-6)mol·L~(-1)；诺氟沙星和洛美沙星的检出限分别是5.03×10~(-9)mol·L~(-1)和7.58×10~(-9)mol·L~(-1)；RSD均在5%以下。方法简单，灵敏度高，用于牛奶样品中NFLX和LFLX的同时测定，结果满意。本文对共发光的反应机制和荧光增强的机理进行了探讨。 第三章根据诺氟沙星的分子结构中喹诺酮能够吸收短波长的光，发出较长 波长的荧光的特征，同时利用稀土元素钇(Ⅲ)与NFLX形成配合物，能使其荧光强度显著增加。因此，建立钇(Ⅲ)离子增敏测定痕量诺氟沙星的分析方法。 在优化的实验条件下，用1cm石英比色池在激发和发射波长分别为275nm和429nm处测定其荧光强度；诺氟沙星在5.10×10~(-9)~5.64×10~(-6)mol·L~(-1)浓度范围内与体系的荧光强度呈良好的线性关系，相关系数为0.9993，检出限为1.52×10~(-9)mol·L~(-1)(S/N=3)；同时试验了常见金属离子及有机物质对其测定的干扰，进行了在牛奶样品和药物胶囊样品的回收试验，回收率在94.0%~105.0%之间，RSD在5%以内，结果令人满意。该方法操作简单、检测限低的特点。 第四章在盐酸介质中，罗丹明G (Rhodamine G, RhG)的分子共振荧光信号强，发射峰尖而对称，受干扰因素少。基于亚硝酸根能催化KBrO_3氧化RhG的反应，建立了催化动力学共振荧光分析法测定痕量NO2-。考察了体系荧光强度减弱值(ΔF)的影响因素，优化了反应条件。最大共振荧光峰位于540nm波长处，NO_2-在4.20~56.00μg·L~(-1)范围内与ΔF呈良好的线性关系，方法检出限为1.65μg·L~(-1)。本方法用于环境水样中NO_2-的测定，RSD小于5.0%，样品加标回收率为98.84%~104.33%。该方法灵敏，结果准确，简便易行，应用于环境水样的检测，结果满意。
[Abstract]:In the first chapter, the significance and progress of the hygienic test of norfloxacin, lomefloxacin and nitrite in the environment were introduced, and the norfloxacin, which was established in this paper, was briefly described. The basic principle and the basis for quantitative determination of three new methods for hygienic examination of Lomefloxacin and nitrite. Chapter 2 is the simultaneous determination of two fluoroquinolones antibiotics. The synchronous fluorescence spectra of norfloxacin (NFLX) and lomefloxacin (LFLX) and their first derivative synchronous fluorescence spectra were studied. The interference between them was avoided by zero intersection method. The synchronous fluorescence spectra of norfloxacin and lomefloxacin were determined in HAc-NaAc buffer solution with pH = 4.0 at 160 nm. Furthermore, the synchronous fluorescence spectra of two species of floxacin were treated with the first derivative, and the signal values of the other species were read at 275.0nm and 283.8nm, where the derivative synchronous fluorescence spectra of NFLX and LFLX were zero, respectively. The linear ranges of NFLX and LFLX were 1.68 脳 10 ~ (-8) ~ (-8) and 5.64 脳 10~(-6)mol ~ (-1), respectively. The detection limits of norfloxacin and lomefloxacin were 5.03 脳 10~(-9)mol L ~ (-1) and 7.58 脳 10~(-9)mol ~ (-1), respectively, and the detection limits of norfloxacin and lomefloxacin were less than 5%. The method is simple and sensitive, and has been applied to the simultaneous determination of NFLX and LFLX in milk samples with satisfactory results. The mechanism of co-luminescence and the mechanism of fluorescence enhancement are discussed in this paper. In chapter 3, according to the characteristics of long wavelength fluorescence, quinolones can absorb the light of short wavelength in the molecular structure of norfloxacin. At the same time, the complex of yttrium (鈪

本文编号：1987422