CdS纳米粒子修饰的恩诺沙星膜电极的制备及性能研究

发布时间：2018-09-14 20:01

【摘要】：目的恩诺沙星(ENR)为第三代氟喹诺酮类合成抗菌药,是动物专用抗生素的一种,具有广谱抗菌性,因此被广泛用于家畜饲养和水产业的鱼类养殖。然而,过量使用恩诺沙星可导致其残留于动物类食品中,进而对人类健康造成危害。此外,微量的恩诺沙星沉积于土壤后具有生态毒性。目前国内外常用于检测动物源性食品中恩诺沙星的方法有高效液相色谱法、酶联免疫法、毛细管电泳法等。这些检测方法成本较高,操作繁琐,前处理复杂,应用条件受到局限。因此建立一种快速简便的恩诺沙星含量检测方法显得十分必要,本文制备了CdS纳米粒子修饰的涂丝型膜电极,并建立电位分析法用于检测药物含量。方法分别以六碘合铋离子和四苯硼钠与恩诺沙星形成缔合物,制备两种不同的缔合物作为电活性物。将这两种电活性物制成不同材质的电极,并筛选出具有能斯特响应的、性能良好的恩诺沙星选择电极。在此基础上,为提高普通恩诺沙星电极的性能,将CdS纳米粒子应用于制备纳米粒子修饰的恩诺沙星电极。建立电化学方法对电极各项性能进行测定,最终将电极应用于猪饲料和猪肉中恩诺沙星含量的测定。结果普通涂丝型离子选择电极的线性响应范围为1.0×10-1~1.0×10~(-5) mol/L,级差电位为26m V/p C,检测下限为8.9×10~(-6) mol/L。将普通涂丝型膜电极应用于猪饲料样品的检测,其RSD小于3.7%。CdS纳米粒子修饰的涂丝型膜电极的Nernst响应范围为1.0×10~(-2)~1.0×10~(-6) mol/L,级差电位为45 m V/p C,其检测下限为7.4×10~(-7)mol/L,且该电极的使用寿命比普通电极长两周,可达12周,在1.0×10-1mol/L~1.0×10~(-4) mol/L恩诺沙星溶液中响应时间小于10 s,在1.0×10~(-5)mol/L~1.0×10~(-7) mol/L恩诺沙星溶液中响应时间小于35 s。采用标准加入法测定CdS修饰膜电极的回收率为96.7%~104.9%。将该电极应用于猪肉样品中恩诺沙星的检测,结果与标准方法对比无显著性差异。结论本文制备了两种普通的涂丝型离子选择电极和CdS纳米粒子修饰的涂丝型膜电极,结果表明所制备的电极均能应用于实际样品检测。其中CdS修饰膜电极的线性响应范围更宽、级差更高、检测下限更低、响应时间更短且p H适用范围更广,其性能优于普通膜电极,为电极性能的优化方法和实际样品中恩诺沙星的快速检测提供一定参考。
[Abstract]:Objective enrofloxacin (ENR) is a synthetic antibiotic of the third generation fluoroquinolones. It is one of the special antibiotics for animals and has broad spectrum antibacterial properties, so it is widely used in livestock breeding and fish breeding in aquaculture. However, excessive use of enrofloxacin can lead to its residues in animal foods, thereby posing a health hazard to humans. In addition, the trace amount of enrofloxacin deposited in soil is ecotoxic. At present, the methods used in the detection of enrofloxacin in animal food are high performance liquid chromatography (HPLC), enzyme-linked immunosorbent assay (Elisa), capillary electrophoresis and so on. These detection methods have high cost, complicated operation, complicated pretreatment and limited application conditions. Therefore, it is necessary to establish a rapid and simple method for the determination of enrofloxacin content. In this paper, the coated membrane electrode modified with CdS nanoparticles was prepared, and the potential analysis method was established for the determination of drug content. Methods two kinds of association complexes of bismuth hexaiodide and sodium tetraphenylboron were prepared with enrofloxacin as electroactive compounds. The electrodes with different materials were prepared from these two kinds of electroactive compounds, and an enrofloxacin selective electrode with Nernst response was selected. On this basis, in order to improve the performance of common enrofloxacin electrode, CdS nanoparticles were used to prepare enrofloxacin modified electrode. An electrochemical method was established to determine the properties of the electrode. Finally, the electrode was applied to the determination of enrofloxacin in pig feed and pork. Results the linear response range of ordinary coated wire ion selective electrode was 1.0 脳 10 ~ (-1) mol/L, differential potential of 26 MV / p C and the detection limit of 8.9 脳 10 ~ (-6) mol/L.. The conventional filament-coated electrode was applied to the detection of pig feed samples. Its Nernst response range is 1.0 脳 10 ~ (-2) ~ (-1) mol/L, differential potential of 45 MV / p ~ (-1) C, and the detection limit is 7.4 脳 10 ~ (-7) mol/L,. The service life of the electrode is two weeks longer than that of the ordinary electrode, and it can reach 12 weeks. The response time was less than 10 s in 1.0 脳 10-1mol/L~1.0 脳 10 ~ (-4) mol/L enrofloxacin solution and less than 35 s in 1.0 脳 10 ~ (-5) mol/L~1.0 脳 10 ~ (-7) mol/L enrofloxacin solution. The standard addition method was used to determine the recovery rate of CdS modified membrane electrode was 96. 7% and 104.9%. The electrode was applied to the determination of enrofloxacin in pork samples. Conclusion in this paper, two kinds of common coated ion selective electrodes and CdS nanoparticles modified coated membrane electrodes have been prepared. The results show that the prepared electrodes can be used for the detection of practical samples. Among them, the linear response range of CdS modified membrane electrode is wider, the level difference is higher, the detection limit is lower, the response time is shorter and the pH range is wider, and its performance is better than that of ordinary membrane electrode. It provides a reference for the optimization of electrode performance and the rapid detection of enrofloxacin in real samples.
【学位授予单位】：锦州医科大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：S859.84

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