Department of Analytical Chemistry, Faculty of Pharmacy, Istanbul University, 34416 Istanbul, Turkey.
Spectrochim Acta A Mol Biomol Spectrosc. 2010 Sep 15;77(1):324-9. doi: 10.1016/j.saa.2010.05.031. Epub 2010 May 31.
A sensitive, simple and rapid spectrophotometric method was developed for the determination of diphenhydramine in pharmaceutical preparation. The method was based on the charge-transfer complex of the drug, as n-electron donor, with 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ), as pi-acceptor. The formation of this complex was also confirmed by UV-vis, FTIR and (1)H NMR spectra techniques and thermal analysis. The proposed method was validated according to the ICH guidelines with respect to linearity, limit of detection, limit of quantification, accuracy, precision, recovery and robustness. The linearity range for concentrations of diphenhydramine was found to be 12.5-150 microg/mL with acceptable correlation coefficients. The detection and quantification limits were found to be 2.09 and 6.27 microg/mL, respectively. The proposed and references methods were applied to the determination of drug in syrup. This preparation were also analyzed with an reference method and statistical comparison by t- and F-tests revealed that there was no significant difference between the results of the two methods with respect to mean values and standard deviations at the 95% confidence level.
建立了一种灵敏、简单、快速的分光光度法测定药物制剂中苯海拉明的含量。该方法基于药物作为供体与 2,3-二氯-5,6-二氰基-1,4-苯醌(DDQ)作为受体之间的电荷转移络合物。通过紫外可见光谱、傅里叶变换红外光谱和(1)H NMR 光谱技术以及热分析也证实了这种络合物的形成。该方法根据 ICH 指南进行了线性、检测限、定量限、准确度、精密度、回收率和稳健性的验证。苯海拉明浓度的线性范围为 12.5-150 μg/mL,相关系数可接受。检测限和定量限分别为 2.09 和 6.27 μg/mL。所提出的方法和参考方法均应用于糖浆中药物的测定。该制剂也用参考方法进行了分析,并通过 t-检验和 F-检验进行了统计学比较,结果表明,在 95%置信水平下,两种方法的平均值和标准偏差之间没有显著差异。