Prashanth Kudige Nagaraju, Basavaiah Kanakapura
Department of Chemistry, University of Mysore, Manasagangotri, Mysore 570006, Karnataka, India.
Acta Pol Pharm. 2012 Mar-Apr;69(2):213-23.
Three rapid, selective and sensitive spectrophotometric methods have been proposed for the quantitative determination of atenolol (ATN) in pure form as well as in its pharmaceutical formulation. The methods are based on charge transfer complexation reaction of ATN as n-electron donor with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), 2,4-dinitrophenol (DNP) and 2,4,6-trinitrophenol (picric acid; PA) as pi-acceptors to give highly colored radical anion species. The colored products were quantified spectrophotometrically at 590 nm with DDQ (method A) and at 420 nm with both DNP (method B) and PA (method C). Under the optimized experimental conditions, Beer's law is obeyed over the concentration ranges of 3-48, 2-24 and 1.5-18 μg/mL ATN for method A, method B and method C, respectively. The molar absorptivity, Sandell sensitivity, limits of detection and quantification are also reported. The effects of reaction medium, reaction time and reagent concentration on the sensitivity and stability of the complexes formed have been examined. The proposed methods were successfully applied to the determination of ATN in pure form and commercial tablets with good accuracy and precision. Statistical comparison of the results was performed using Student's t-test and F-ratio at 95% confidence level and the results showed no significant difference between the reference and proposed methods with regard to accuracy and precision. Further, the accuracy and reliability of the methods were confirmed by recovery studies via standard addition technique.
已提出三种快速、选择性和灵敏的分光光度法,用于定量测定纯阿替洛尔(ATN)及其药物制剂中的阿替洛尔。这些方法基于阿替洛尔作为n电子供体与作为π受体的2,3-二氯-5,6-二氰基-1,4-苯醌(DDQ)、2,4-二硝基苯酚(DNP)和2,4,6-三硝基苯酚(苦味酸;PA)发生电荷转移络合反应,生成颜色很深的自由基阴离子物种。用DDQ时在590 nm处(方法A),用DNP和PA时在420 nm处(方法B和方法C)对有色产物进行分光光度法定量。在优化的实验条件下,方法A、方法B和方法C中阿替洛尔的浓度范围分别在3 - 48、2 - 24和1.5 - 18 μg/mL时符合比尔定律。还报道了摩尔吸光率、桑德尔灵敏度、检测限和定量限。研究了反应介质、反应时间和试剂浓度对所形成络合物的灵敏度和稳定性的影响。所提出的方法已成功应用于纯阿替洛尔和市售片剂中阿替洛尔的测定,具有良好的准确度和精密度。使用学生t检验和F比在95%置信水平下对结果进行统计比较,结果表明在准确度和精密度方面,参考方法和所提出的方法之间没有显著差异。此外,通过标准加入技术进行回收率研究,证实了这些方法的准确度和可靠性。