Ciltas Ulvihan, Yilmaz Bilal, Kaban Selcuk, Akcay Bilge Kaan, Nazik Gulsah
Department of Analytical Chemistry, School of Pharmacy, Ataturk University, Erzurum, Turkey.
Iran J Pharm Res. 2015 Summer;14(3):715-22.
In this study, a simple and reliable square wave voltammetric (SWV) method was developed and validated for determination of diclofenac in pharmaceutical preparations and human serum. The proposed method was based on electrooxidation of diclofenac at platinum electrode in 0.1 M TBAClO4/acetonitrile solution. The well-defined two oxidation peaks were observed at 0.87 and 1.27 V, respectively. Calibration curves that were obtained by using current values measured for second peak were linear over the concentration range of 1.5-17.5 μg mL(-1) and 2-20 μg mL(-1) in supporting electrolyte and serum, respectively. Precision and accuracy were also checked in all media. Intra- and inter-day precision values for diclofenac were less than 3.64, and accuracy (relative error) was better than 2.49%. Developed method in this study is accurate, precise and can be easily applied to Diclomec, Dicloflam and Voltaren tablets as pharmaceutical preparation. Also, the proposed technique was successfully applied to spiked human serum samples. No electroactive interferences from the endogenous substances were found in human serum.
在本研究中，开发并验证了一种简单可靠的方波伏安法（SWV），用于测定药物制剂和人血清中的双氯芬酸。该方法基于双氯芬酸在0.1 M TBAClO4/乙腈溶液中的铂电极上进行电氧化。分别在0.87 V和1.27 V处观察到明确的两个氧化峰。使用第二个峰测量的电流值得到的校准曲线在支持电解质和血清中的浓度范围分别为1.5 - 17.5 μg mL(-1)和2 - 20 μg mL(-1)时呈线性。还在所有介质中检查了精密度和准确度。双氯芬酸的日内和日间精密度值均小于3.64，准确度（相对误差）优于2.49%。本研究中开发的方法准确、精密，可轻松应用于作为药物制剂的双氯灭痛、双氯芬乳膏和扶他林片剂。此外，所提出的技术已成功应用于加标的人血清样品。在人血清中未发现内源性物质的电活性干扰。
