Abstract

A simple, economical and selective method employing ion pair dispersive liquid−liquid microextraction (DLLME) coupled with spectrophotometric determination of carbamazepine (CBZ) in pharmaceutical preparations and biological samples was developed. The method is based on reduction of Mo(VI) to Mo(V) using a combination of ammonium thiocyanate and ascorbic acid in acidic medium to form a red binary Mo(V) thiocyanate complex. After addition of CBZ to the complex, extraction of the formed CBZ−Mo(V)−(SCN)₆ was performed using a mixture of methylene chloride and methanol. Then, the measurement of target complex was performed at the wavelength of 470 nm. The important extraction parameters affecting the efficiency of DLLME were studied and optimized in detail. At the optimum conditions, the linear range was 0.02–0.2 µg/mL. Moreover, the limits of detection and quantification were 0.01 and 0.04 µg/mL, respectively. High enrichment factor was obtained (118). Good recoveries at 0.06, 0.15 and 0.2 µg/mL ranging from 93 to 102% were achieved. The proposed method was successfully applied to the determination of CBZ in pharmaceutical formulations and biological samples.

中文翻译：

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离子对分散液微萃取结合分光光度法测定卡马西平的药物制剂和生物样品

摘要

开发了一种简单，经济，选择性的方法，该方法采用离子对分散液-液微萃取（DLLME）结合分光光度法测定药物制剂和生物样品中的卡马西平（CBZ）。该方法基于在酸性介质中使用硫氰酸铵和抗坏血酸的组合将Mo（VI）还原为Mo（V），形成红色的二元Mo（V）硫氰酸盐络合物。将CBZ添加到配合物中后，提取形成的CBZ-Mo（V）-（SCN）₆使用二氯甲烷和甲醇的混合物进行。然后，在470nm的波长下进行目标复合物的测量。研究并优化了影响DLLME效率的重要提取参数。在最佳条件下，线性范围为0.02–0.2 µg / mL。此外，检测限和定量限分别为0.01和0.04 µg / mL。获得了高富集因子（118）。在0.06、0.15和0.2 µg / mL的93至102％范围内实现了良好的回收率。该方法成功地用于药物制剂和生物样品中CBZ的测定。