Rajendraprasad Nagaraju, Basavaiah Kanakapura, Vinay Kanakapura Basavaiah
Acta Chim Slov. 2011 Sep;58(3):621-8.
Two cerimetric procedures are described for the assay of oxcarbazepine (OXC) in bulk drug and in tablets. Titrimetry (method A) is based on the reaction of OXC by a measured excess cerium(IV) sulphate in sulphuric acid medium and the determination of the unreacted oxidant by titration with iron(II) solution using ferroin as indicator. Spectrophotometry (method B) is based on oxidation of OXC by cerium(IV) in perchloric acid (HClO4) medium and the determination of the unreacted oxidant using a colour reaction with p-dimethylaminobenzaldehyde (p-DMAB) having an absorption maximum of 460 nm. The titrimetric method is applicable in the range of 2.0-20.0 mg OXC with a 1:2 reaction stoichiometry [OXC:Ce(IV)]. In the spectrophotometric method a rectilinear relationship is obtained over the concentration range of 0.3-6.0 µg mL-1 OXC. The linear regression equation of the calibration graph is A = 0.9820-0.1477 C with a regression coefficient (r) of -0.9967 (n = 6). The molar absorptivity is calculated to be 3.76 × 104 L mol-1 cm-1 and the Sandell sensitivity is 0.0067 µg cm-2. The limits of detection (LOD) and quantification (LOQ) values are calculated according to ICH guidelines. The methods are successfully applied to the determination of OXC in tablets.
本文描述了两种用于测定原料药和片剂中奥卡西平(OXC)的铈量法。滴定法(方法A)基于在硫酸介质中,奥卡西平与过量的硫酸铈(IV)反应,然后用亚铁溶液滴定未反应的氧化剂,以邻二氮菲亚铁为指示剂。分光光度法(方法B)基于在高氯酸(HClO4)介质中,奥卡西平被铈(IV)氧化,然后利用与对二甲氨基苯甲醛(p-DMAB)的显色反应测定未反应的氧化剂,该显色反应的最大吸收波长为460nm。滴定法适用于2.0 - 20.0mg奥卡西平的测定,反应化学计量比为1:2 [奥卡西平:铈(IV)]。在分光光度法中,奥卡西平浓度在0.3 - 6.0μg mL-1范围内呈线性关系。校准曲线的线性回归方程为A = 0.9820 - 0.1477C,回归系数(r)为 - 0.9967(n = 6)。计算得到摩尔吸光系数为3.76×104 L mol-1 cm-1,桑德尔灵敏度为0.0067μg cm-2。根据ICH指南计算检测限(LOD)和定量限(LOQ)值。这些方法成功应用于片剂中奥卡西平的测定。