Darwish Ibrahim A, Khedr Alaa S, Askal Hassan F, Mohamed Ramadan M
Assiut University, Faculty of Pharmacy, Department of Pharmaceutical Analytical Chemistry, Assiut 71526, Egypt.
J AOAC Int. 2006 Mar-Apr;89(2):341-51.
Eight spectrophotometric methods for determination of ribavirin have been developed and validated. These methods were based on the oxidation of the drug by different inorganic oxidants: ceric ammonium sulfate, potassium permanganate, ammonium molybdate, ammonium metavanidate, chromium trioxide, potassium dichromate, potassium iodate, and potassium periodate. The oxidation reactions were performed in perchloric acid medium for ceric ammonium sulfate and in sulfuric acid medium for the other reagents. With ceric ammonium sulfate and potassium permanganate, the concentration of ribavirin in its samples was determined by measuring the decrease in the absorption intensity of the colored reagents at 315 and 525 nm, respectively. With the other reagents, the concentration of ribavirin was determined by measuring the intensity of the developed colored reaction products at the wavelengths of maximum absorbance: 675, 780, 595, 595, 475, and 475 nm for reactions with ammonium molybdate, ammonium metavanidate, chromium trioxide, potassium dichromate, potassium iodate, and potassium periodate, respectively. Different variables affecting the reaction conditions were carefully studied and optimized. Under the optimum conditions, linear relationships with good correlation coefficients (0.9984-0.9998) were found between the absorbance readings and the concentrations of ribavirin in the range of 4-1400 microg/mL. The molar absorptivities were correlated with the oxidation potential of the oxidants used. The precision of the methods were satisfactory; the values of relative standard deviation did not exceed 1.64%. The proposed methods were successfully applied to the analysis of ribavirin in pure drug material and capsules with good accuracy and precision; the recovery values were 99.2-101.2 +/- 0.48-1.30%. The results obtained using the proposed spectrophotometric methods were comparable with those obtained with the official method stated in the United States Pharmacopeia.
已开发并验证了八种分光光度法测定利巴韦林。这些方法基于药物被不同无机氧化剂氧化:硫酸铈铵、高锰酸钾、钼酸铵、偏钒酸铵、三氧化铬、重铬酸钾、碘酸钾和高碘酸钾。氧化反应在高氯酸介质中对硫酸铈铵进行,对其他试剂在硫酸介质中进行。对于硫酸铈铵和高锰酸钾,分别通过测量有色试剂在315和525nm处吸收强度的降低来测定样品中利巴韦林的浓度。对于其他试剂,通过测量显色反应产物在最大吸收波长处的强度来测定利巴韦林的浓度:与钼酸铵、偏钒酸铵、三氧化铬、重铬酸钾、碘酸钾和高碘酸钾反应时,分别为675、780、595、595、475和475nm。仔细研究并优化了影响反应条件的不同变量。在最佳条件下,在4 - 1400μg/mL范围内,吸光度读数与利巴韦林浓度之间发现了具有良好相关系数(0.9984 - 0.9998)的线性关系。摩尔吸光率与所用氧化剂的氧化电位相关。这些方法的精密度令人满意;相对标准偏差值不超过1.64%。所提出的方法成功应用于原料药和胶囊中利巴韦林的分析,具有良好的准确度和精密度;回收率值为99.2 - 101.2±0.48 - 1.30%。使用所提出的分光光度法获得的结果与美国药典中规定的法定方法获得的结果相当。