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在碱性条件下,利用Cu~(2+)对鲁米诺-H_2O_2化学发光体系的催化作用和双酚A对该体系的化学发光信号具有明显抑制的作用,结合流动注射技术建立了测定双酚A的新方法。在单因素试验的基础上,利用响应曲面对化学发光测定双酚A条件参数进行优化研究,选择Cu~(2+)浓度、鲁米诺以及H_2O_2为自变量,化学发光强度为响应值,采用Box-Behnken设计方法,研究各自变量及其交互作用对化学发光强度的影响,利用Design Expert软件对数据进行回归分析,得到二次多项式回归方程的预测模型。在最佳实验条件下,双酚A的浓度在0.10~10μmol/L范围内与相对化学发光强度呈良好线性关系,线性方程ΔI=214.29×10~6c-200.41(r=0.9991),方法的检出限为50 nmol/L,相对偏差为1.9%。对实际样品中的双酚A含量进行测定,回收率在95%~105%,并并对化学发光机理进行了研究。
Under alkaline conditions, the catalytic effect of Cu 2+ on the luminol-H 2 O 2 chemiluminescence system and the inhibition of the chemiluminescence signal of the system by bisphenol A were significantly inhibited. Combined with the flow-injection technique, A new method of phenol A On the basis of single factor experiments, the response surface was used to optimize the conditions of bisphenol A chemiluminescence determination. Cu 2+ concentration, luminol and H 2 O 2 were chosen as independent variables. The chemiluminescence intensity was the response value, The Box-Behnken design method was used to study the influence of each variable and its interaction on the chemiluminescence intensity. The regression analysis was conducted by using Design Expert software to obtain the prediction model of quadratic polynomial regression equation. Under the optimal experimental conditions, the concentration of bisphenol A showed a good linear relationship with the relative chemiluminescence intensity in the range of 0.10 ~ 10μmol / L, the linear equation ΔI = 214.29 × 10 ~ 6c-200.41 (r = 0.9991) The limit was 50 nmol / L with a relative deviation of 1.9%. The actual sample of bisphenol A content determination, the recovery rate of 95% to 105%, and the mechanism of chemiluminescence was studied.