Rezaei B, Mokhtari A
Department of Chemistry, Isfahan University of Technology, Isfahan 84156 IR, Iran.
Luminescence. 2008 Nov-Dec;23(6):357-64. doi: 10.1002/bio.1040.
The main purpose of this study was to develop an inexpensive, simple, rapid and sensitive chemiluminescence (CL) method for the determination of enrofloxacin (ENRO) using a flow-injection system. This method is based on rapid reduction of Ru(phen)(3)(3+), which is produced in the reaction between Ru(phen)(3)(2+) and acidic Ce(IV) by ENRO, producing strong CL. A central composite design (CCD) was used for optimization of the chemical variables. Regression analysis of the data from the CCD demonstrated that a second-order polynomial model is an adequate description of the surface over the factor limits studied. Optimization using CCD gave approximately four-fold better results than the single-factor-at-a-time method. Under optimal experimental conditions, the CL response was proportional to the concentration of ENRO over a wide range (0.008-3.6 microg/mL) with a correlation coefficient of 0.9986 and a detection limit of 0.003 microg/mL (3sigma). The relative standard deviation for 11 repeated determinations of 0.14 microg/mL ENRO was 4.2%. This method was successfully applied to the analysis of commercial formulations, spiked plasma and spiked poultry tissue. Sample analyses showed good recovery percentages for drugs and spiked plasma (95.1-103.9%). Recovery percentages for spiked poultry tissue were in the range 77.6-87.3%. The minimum sampling rate was 100 samples/h.
本研究的主要目的是开发一种使用流动注射系统测定恩诺沙星(ENRO)的廉价、简单、快速且灵敏的化学发光(CL)方法。该方法基于ENRO使Ru(phen)(3)(2+)与酸性Ce(IV)反应生成的Ru(phen)(3)(3+)快速还原,产生强烈的化学发光。采用中心复合设计(CCD)对化学变量进行优化。对CCD数据的回归分析表明,二阶多项式模型能够充分描述所研究因子范围内的表面情况。使用CCD进行优化得到的结果比一次单因素法大约好四倍。在最佳实验条件下,化学发光响应在较宽浓度范围(0.008 - 3.6 μg/mL)内与ENRO浓度成正比,相关系数为0.9986,检测限为0.003 μg/mL(3σ)。对0.14 μg/mL ENRO进行11次重复测定的相对标准偏差为4.2%。该方法成功应用于市售制剂、加标血浆和加标家禽组织的分析。样品分析显示药物和加标血浆的回收率良好(95.1 - 103.9%)。加标家禽组织的回收率在77.6 - 87.3%范围内。最低采样率为100个样品/小时。