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采用掺硼金刚石电极的伏安法测定药物制剂和人尿中的青霉素 V。

Voltammetric determination of penicillin V in pharmaceutical formulations and human urine using a boron-doped diamond electrode.

机构信息

Institute of Analytical Chemistry, Faculty of Chemical and Food Technology, Slovak University of Technology, Radlinského 9, Bratislava, SK-812 37, Slovak Republic.

出版信息

Bioelectrochemistry. 2012 Dec;88:36-41. doi: 10.1016/j.bioelechem.2012.04.004. Epub 2012 Apr 24.

Abstract

Simple, sensitive and selective differential pulse voltammetric method for determination of penicillin V on a bare (unmodified) boron-doped diamond electrode has been developed. Penicillin V provided highly reproducible and well-defined irreversible oxidation peak at very positive potential of +1.6V (vs. Ag/AgCl). The optimum experimental conditions for oxidation of penicillin V were achieved in acetate buffer solution (pH 4.0). The modulation amplitude of 0.1V, modulation time of 0.05s and scan rate of 0.05Vs(-1) were selected as optimum instrumental parameters for differential pulse voltammetry. Linear response of peak current on the concentration in the range from 0.5 to 40μM with coefficient of determination of 0.999, good repeatability (RSD of 1.5%) and detection limit of 0.25μM were observed without any chemical modifications and electrochemical surface pretreatment. The effect of possible interferents such as stearic acid, glucose, urea, uric acid and ascorbic acid appeared to be negligible which evidently proved the good selectivity of method. The practical analytical utility of proposed method was demonstrated by determination of penicillin V in pharmaceutical formulations (tablets) and human urine samples with satisfactory recoveries (from 98 to 101% for tablets and 97 to 103% for human urine).

摘要

已经开发出了一种简单、灵敏和选择性的差分脉冲伏安法,用于在裸(未修饰)掺硼金刚石电极上测定青霉素 V。青霉素 V 在非常正的电位+1.6V(相对于 Ag/AgCl)处提供了高度重现性和定义良好的不可逆氧化峰。在醋酸盐缓冲溶液(pH 4.0)中实现了青霉素 V 氧化的最佳实验条件。选择 0.1V 的调制幅度、0.05s 的调制时间和 0.05Vs(-1) 的扫描速率作为差分脉冲伏安法的最佳仪器参数。在 0.5 至 40μM 的浓度范围内,峰电流与浓度呈线性关系,相关系数为 0.999,具有良好的重复性(RSD 为 1.5%)和检测限为 0.25μM,无需任何化学修饰和电化学表面预处理。观察到可能的干扰物(如硬脂酸、葡萄糖、尿素、尿酸和抗坏血酸)的影响可以忽略不计,这显然证明了该方法的良好选择性。该方法的实际分析应用通过测定药物制剂(片剂)和人尿样中的青霉素 V 得到了证明,回收率令人满意(片剂为 98%至 101%,人尿为 97%至 103%)。

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