以导电碳黑糊电极为工作电极,研究了结晶紫(CT)和盐酸环丙沙星(CPFX)的伏安行为,结果表明,B-R缓冲溶液(pH 4.5)中,二者具有互不干扰的灵敏电极响应.实验对缓冲液种类、pH、富集电位和富集时间等影响检测的因素进行了研究与优化,进而建立了二者的伏安检测方法.采用半微分脉冲模式,CPFX共存情况下,CT的氧化峰电流与其浓度在2.5×10^-8~ 1.325 ×10^-6 mol/L范围内呈线性关系;CT共存情况下,CPFX的氧化峰电流与其浓度在5.0×10^-8~4.85×10^-6mol/L范围内呈线性关系;检测限(S/N=3)分别为10.5和21.2 nmol/L.将所建立的电化学方法应用于测定淡水渔业水样中CT和CPFX的残留量,得到了较满意的结果.CT和CPFX的平均回收率分别为97.8%和101.1%.该方法具有操作简便、响应快和成本低等显著优点,因而具有潜在推广应用价值.
The voltammetric behaviors of Crystal violet (CT) and Ciprofloxacin hydrochloride (CPFX) were studied at the conductive carbon paste electrode. Results demonstrated that in B - R buffer solution of pH 4.5 the two molecules displayed non -interfering sensitive electrochemical responses. The experiment has conducted research and optimization of such factors which influence the detection as the buffer solution category, pH, accumulation potential and time. And then a newmethod for determining residual CT and CPFX was developed. Tested with half impulsive differential mode, there was a linear relationship between the peak currents and the concentration of CT in the range of 2.5 ×10^-5 - 1. 325×10^-6mol/L with a coexistence of CPFX; there was a linear relationship between the peak currents and the concentration of CPFX in the range of 5.0 ×10^-5 - 4.85 ×10^ -6 mol/L with a coexistence of CT. The detection limits were 10.5 and 21.2 nmolfL ( S/N= 3 ), respectively. Satisfactory results were obtained when the new method was used to measure CT and CPFX in the real fresh fishery water samples with average recovery rates of 97.8% and 101.1%, respectively. The method exhibits many attractive advantages, such as simple operation, rapid response, low cost, and so on. Therefore it is promising for popular application. [ Chinese Fishery Quality and Stand- ards, 2015, 5(3):27-33]