非现场型红外光谱法在电化学检测己烯雌酚中的应用

建立了亚甲基蓝(MB)修饰多壁碳纳米管玻碳电极(MWNT/GCE)测定药片中己烯雌酚(DES)的方法,并采用非现场型傅里叶红外光谱技术(Off-site-FTIR)对亚甲基蓝修饰电极进行了表征检测.结果表明,聚亚甲基蓝在电极上的形成是由于双键断裂,使得在1603.3cm-1处的C＝N键伸缩振动吸收带消失;在0.2mol/L的磷酸缓冲液(pH=7.5)中,采用修饰电极己烯雌酚的伏安曲线出现特征氧化峰,峰电位为0.209V,峰电流显著提高,表现出明显的电催化作用;利用方波伏安法(Square Ware Voltammetry,SWV)测得峰电流与己烯雌酚质量浓度在1.0×10-5-1.0×10-9g/L范围内呈线性关系,线性相关系数0.9949,检出限5.0× 10-10g/L.用此法对己烯雌酚药片的含量进行了测定,测定结果与标示相符.

Application of Electrochemical Detection of Diethylstilbestrol by Off-Site Infrared Spectroscopy

The method for the determination of diethylstilbestrol（DES） in tablets by methylene blue（MB） modified multi-walled carbon nanotubes-glassy carbon electrode（MWNT/GCE） was established.The MB modified electrode was characterized and detected by off-site-FTIR technology. The experimental results showed that because of the double bond fracturing,C =N bond telescopic vibration absorption belt disappeared at 1603.3cm^-1.The current voltage characteristic cure of DES exhibited a well-defined and sensitive oxidation peak at this modified electrode in 0.2mol/L PBS buffer（pH of 7.5）,and the oxidation peak potential was 0.209V,and the peak current significantly enhanced.It was shown that this electrode exhibited a significant catalytic.effect toward the oxidation of DES.The oxidation peak current was linear relation with the concentration of DES in the range of 1.0×10^-5—1.0×10^-9g/L with the correlation coefficient of 0.9949 and the detection limit of 5.0×10^-10g/L by square ware voltammetry（SWV）.The proposed method was used to determine DES tablets,and the results was consistent with the marked.