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作 者:廖羽 余兰 Liao Yu;Yu Lan(Department of Analytical Chemistry,School of Pharmacy,Zunyi Medical University,Zunyi Guizhou 563099,China)
机构地区:[1]遵义医科大学药学院分析化学教研室,贵州遵义563099
出 处:《遵义医科大学学报》2020年第1期104-111,共8页Journal of Zunyi Medical University
基 金:国家自然科学基金资助项目(NO:21768006)。
摘 要:目的建立荷移分光光度法测定西咪替丁的含量。方法采用西咪替丁与2,3-二氯-5,6-二氰基对苯醌进行荷移反应,以聚氧乙烯蓖麻油EL-40作为增敏剂,对反应物用量、反应时间、反应温度等条件进行考察,确定反应的最佳条件。对形成荷移络合物的反应机理进行了研究。结果在乙腈介质中,电子给予体西咪替丁与电子受体2,3-二氯-5,6-二氰基对苯醌在室温下形成1∶1型荷移络合物,最大吸收波长458 nm,摩尔吸光系数为2.9×10^3 L/(mol·cm);线性范围10.00~80.00μg/mL,相关系数r=0.9995,检测限和定量限分别为2.07、6.28μg/mL;重复性和日间精密度的RSD分别为0.90%、0.94%;本方法测定片剂、胶囊中的西咪替丁含量,结果与药典方法无显著性差异,其回收率为98.98%~101.63%和98.00%~101.60%。结论该方法结果准确、重现性好,可用于西咪替丁片剂和胶囊剂的质量控制。Objective A charge transfer spectrophotometry was established for the determination of cimetidine.Methods The charge transfer reaction between cimetidine and 2,3-dichloro-5,6-dicy ano-1,4-benzoquinore was carried out and sensitized by the polyoxyethylene castor oil EL-40.The reactant dosage,reaction time and temperature were investigated to establish the optimum reaction conditions.Results In acetonitrile medium,cimetidine as the electron donor and 2,3-dichloro-5,6-dicyano-1,4-benzoquinore as the electron acceptor formed 1∶1 charge transfer complex at room temperature with apparent molar absorptivity of 2.9×10^3 L/(mol·cm)under 458 nm.Lambert-Beer law was obeyed over the concentration range of 10.00-80.00μg/ml for cimetidine with correlation coefficient of 0.9995.The detection and quantitative limits were 2.07μg/ml and 6.28μg/ml,respectively.The RSD of repeatability and day precision were 0.90%and 0.94%respectively.The reaction mechanism of charge shift complex formation was studied.The determination of cimetidine contained in tablets and capsules by the proposed method showed no significant difference with the pharmacopoeia.The recoveries were 98.98%-101.63%and 98.00%-101.60%.Conclusion The accuracy and precision of the proposed method were satisfactory.The method was successfully applied for analysis of cimetidine in tablets and capsules.
关 键 词:电荷转移反应 分光光度法 西咪替丁 2 3-二氯-5 6-二氰基对苯醌
分 类 号:R917[医药卫生—药物分析学]
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