摘要
基于碱性介质中鲁米诺在石墨烯修饰玻碳电极(GCE)表面的弱电化学发光信号可被少量甲巯咪唑显著增敏的原理建立了一种灵敏测定甲巯咪唑的电化学发光新方法。实验考察了反应介质、石墨烯用量、鲁米诺浓度及电化学扫描速率对体系电化学发光信号的影响。结果发现:在8. 0μL的石墨烯用量、0. 01 mol·L~(-1)NaOH、0. 7μmol·L~(-1)鲁米诺及100 mV/s的扫描速率的优化条件下,甲巯咪唑浓度在6. 0×10~(-8)~1. 0×10~(-5)mol·L~(-1)范围内与其增敏的电化学发光强度呈良好的线性关系,检出限为2. 0×10~(-8)mol·L~(-1),其相对标准偏差(RSD)为3. 5%(c=0. 5μmol·L~(-1),n=11)。该方法可用于甲巯咪唑含量的临床测定,结果较为满意。
A novel electrochemiluminescence(ECL) method was developed for the sensitive detection of methimazole based on the fact that in the alkaline medium,the weak ECL signal of luminol could be significantly enhanced by a little amount of methimazole on the surface of graphene modified glass carbon electrode. The effects of reaction medium,graphene dosage,luminol concentration and electrochemical scanning rates on ECL signal of the selected system were investigated. Results showed that under the optimal contions of 8. 0 μL of graphene amount,0. 01 mol·L~(-1)of sodium hydroxide,0. 7 μmol·L~(-1)of luminol and 100 mV/s of electrochemical scaning rate,the increased ECL intensity for methimazole was linear in the concentration range of 6. 0 × 10~(-8)-1. 0 × 10~(-5)mol·L~(-1)with a detection limit of 2. 0 × 10~(-8)mol·L~(-1)and a relative standard deviation( RSD) of 3. 5%( c = 0. 5μmol·L~(-1),n = 11). The proposed method could be applied in the clinical analysis of methimazole tablets with satisfactory results.
引文
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