论文部分内容阅读
基于米非司酮在碱性条件下对AgNPs-Luminol-H2O2化学发光体系的抑制作用,提出了一种化学发光法测定米非司酮的新方法。结合流动注射分析技术,在采用单一变量法考察实验条件的基础上,利用响应曲面优化法中4因素4水平的Box-Behnken设计优化了该化学发光体系测定米非司酮的有关参数,用Design-Expert的Trial软件对所得结果进行了二次回归拟合,得到数学模型,并利用最小二乘法对该模型的各参数进行了方差分析和统计性检验,结果表明其可以用于预测化学发光强度的实际情况。在最佳实验条件下,米非司酮的化学发光强度与其质量浓度在8.0×10-8~1.0×10-4g/mL范围内呈良好的线性关系,方法的检出限为3.0×10-9g/mL(3σ),相对标准偏差为2.6%(n=11,8.0×10-6g/mL)。方法用于药物制剂及人血清中米非司酮的检测,回收率为97.0%~105.0%,同时对可能的化学发光机理进行了探讨。
Based on the inhibitory effect of mifepristone on AgNPs-Luminol-H2O2 chemiluminescence system under alkaline conditions, a new chemiluminescence method for the determination of mifepristone was proposed. Combining the flow injection analysis technique and the Box-Behnken design with 4 factors and 4 levels in response surface methodology, the parameters of mifepristone in this chemiluminescence system were optimized by single variable method. -Expert’s Trial software to quadratic regression fitting the results obtained, the mathematical model, and the use of least squares method of variance analysis and statistical tests of the parameters of the model, the results show that it can be used to predict the chemiluminescence intensity The actual situation. Under the optimal experimental conditions, the linear relationship between the chemiluminescence intensity of mifepristone and its mass concentration in the range of 8.0 × 10-8 ~ 1.0 × 10-4g / mL showed that the detection limit of the method was 3.0 × 10- 9g / mL (3σ) with a relative standard deviation of 2.6% (n = 11,8.0 × 10-6g / mL). The method was applied to the determination of mifepristone in pharmaceutical preparations and human serum. The recoveries ranged from 97.0% to 105.0%. At the same time, possible chemiluminescence mechanisms were discussed.