Darwish Khaled M, Salama Ismail, Mostafa Samia, El-Sadek Mohamed
Department of Pharmaceutical Chemistry, Suez Canal University, Ismailia, Egypt.
Pak J Pharm Sci. 2012 Jan;25(1):207-17.
An easy, precise and valid extractional-spectrophotometric technique is described for the assessment of metronidazole (MNZ), tinidazole (TNZ), ornidazole (ONZ) and secnidazole (SNZ) in pure state and in their pharmaceutical formulations. The technique includes first the reduction of above cited drugs using HCl and zinc powder, then the formation of intense yellow colored ion-association complex species (1:3 drug/dye) using bromothymol blue (BTB) in a buffered aqueous acidic medium at pH 3-3.50. The colored products are extracted into dichloromethane and quantitatively determined at 416-420 nm. The experimental operating factors influencing the ion-pairs development were studied and optimized to obtain the maximum color intensity. The Beer plots are obeyed in the concentration ranges 2.50-22.50, 2.50-30, 7.50-35 and 5-30 μgml-1 for MNZ, TNZ, ONZ and SNZ, respectively, with correlation coefficients not less than 0.9995. The proposed technique is recommended for the routine quality control analysis of the investigated drugs in commercial tablets with no observed interference from common pharmaceutical adjuvants. Results of such analysis were statistically validated and through recovery studies, showing excellent agreement with those achieved by the reported techniques.
本文描述了一种简便、精确且有效的萃取分光光度法,用于评估甲硝唑(MNZ)、替硝唑(TNZ)、奥硝唑(ONZ)和塞克硝唑(SNZ)的纯品及其药物制剂。该技术首先使用盐酸和锌粉还原上述药物,然后在pH值为3 - 3.50的缓冲酸性水介质中,用溴百里酚蓝(BTB)形成强烈黄色的离子缔合物络合物(药物/染料比例为1:3)。将有色产物萃取到二氯甲烷中,并在416 - 420 nm处进行定量测定。研究并优化了影响离子对形成的实验操作因素,以获得最大颜色强度。甲硝唑、替硝唑、奥硝唑和塞克硝唑在浓度范围分别为2.50 - 22.50、2.50 - 30、7.50 - 35和5 - 30 μg/ml时符合比尔定律,相关系数不小于0.9995。该方法推荐用于市售片剂中所研究药物的常规质量控制分析,未观察到常见药用辅料的干扰。此类分析结果经统计学验证,并通过回收率研究表明,与报道技术所得结果高度一致。