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利用聚3,4-乙撑二氧噻吩修饰金电极测定药物中异烟肼的新型伏安法的设计与优化

Design and Optimization of a New Voltammetric Method for Determination of Isoniazid by Using PEDOT Modified Gold Electrode in Pharmaceuticls.

作者信息

Demirkaya-Miloglu Fatma, Oznuluer Tuba, Ozdurak Buket, Miloglu Elmas

机构信息

Ataturk University, Faculty of Pharmacy, Department of Analytical Chemistry, 25240 Erzurum/TURKEY.

Ataturk University, Faculty of Chemistry, Department of AnalyticalChemistry, 25240 Erzurum/TURKEY.

出版信息

Iran J Pharm Res. 2016 Winter;15(Suppl):65-73.

Abstract

Isoniazid (INH) was studied with regard to its electrochemical treatment on a strongly alkaline solution of a poly (3,4-ethylenedioxythiophene)-modified gold electrode, using both cyclic voltammetric and controlled potential techniques. Electrocatalytic performance measurements of this composite electrode toward oxidation of INH exhibited an increase of 4-folds in oxidation peak densities compared to the bare gold electrode. Central composite design method was used to obtain optimum experimental conditions, and used critical parameters (pH (A), scan rate (mV/s, B) and temperature (C, C) to assess the effects on amperometric response. Optimum experimental conditions were achieved by using a pH of 9.2 with a scan rate of 260 mV/s and a temperature of 30 C. Under these circumstances, a good linear relationship was observed between peak current densities and INH concentration in the range of 0.05-2 μM, with correlation coefficient of 0.9998. Furthermore, the method was very sensitive (limit of quantitation, 0.0043 μM), accurate (relative error, -5.65 to 4.03) and precise (relative standard deviation %, ≤ 7.97). The method was also applied to determine INH in pharmaceutical formulations, and statistically compared the results with the official method using the two one-sided equivalence test; the results were in good agreement with those obtained by the official and reported methods.

摘要

采用循环伏安法和控制电位技术,研究了异烟肼(INH)在聚(3,4 - 亚乙基二氧噻吩)修饰金电极的强碱性溶液中的电化学处理。与裸金电极相比,该复合电极对INH氧化的电催化性能测量显示氧化峰密度增加了4倍。采用中心复合设计方法获得最佳实验条件,并使用关键参数(pH(A)、扫描速率(mV/s,B)和温度(C,C))来评估对安培响应的影响。通过使用pH为9.2、扫描速率为260 mV/s和温度为30℃实现了最佳实验条件。在这些条件下,在0.05 - 2 μM范围内观察到峰电流密度与INH浓度之间具有良好的线性关系,相关系数为0.9998。此外,该方法非常灵敏(定量限,0.0043 μM)、准确(相对误差,-5.65至4.03)且精密度高(相对标准偏差%,≤ 7.97)。该方法还应用于药物制剂中INH的测定,并使用双侧等效性检验将结果与官方方法进行统计学比较;结果与官方方法和报道方法获得的结果高度一致。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/88a6/5242353/2c96e5d0d25d/ijpr-15-065-g001.jpg

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