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使用N-溴代琥珀酰亚胺作为溴化剂测定原料药和片剂中的琥珀酸舒马曲坦。

Utilization of N-bromosuccinimide as a brominating agent for the determination of sumatriptan succinate in bulk drug and tablets.

作者信息

Prashanth Kudige N, Basavaiah Kanakapura, Raghu Madihalli S

机构信息

Department of Chemistry, University of Mysore, Manasagangotri, Mysore, Karnataka 570006, India.

出版信息

Int J Anal Chem. 2013;2013:934357. doi: 10.1155/2013/934357. Epub 2013 Jul 9.

Abstract

One titrimetric and two spectrophotometric methods which are simple, sensitive, and economic are described for the determination of sumatriptan succinate (STS) in bulk drug and in tablet dosage form using N-bromosuccinimide (NBS) as a brominating agent. In titrimetry, aqueous solution of STS is treated with a measured excess of NBS in acetic acid medium, and after the bromination of STS is judged to be complete, the unreacted NBS is determined iodometrically (method A). Spectrophotometric methods entail addition of a known excess of NBS in acid medium followed by the determination of residual NBS by its reaction with excess iodide, and the liberated iodine (I3 (-)) is either measured at 370 nm (method B) or liberated iodine is reacted with starch followed by the measurement of the blue colored starch-iodine complex at 570 nm (method C). Titrimetric method is applicable over range 1.0-10.0 mg STS (method A), and the reaction stoichiometry is found to be 1 : 3 (STS : NBS). The spectrophotometric methods obey Beer's law for concentration range 0.6-15.0  μ g mL(-1) (method B) and 0.2-4.0  μ g mL(-1) (method C). The calculated apparent molar absorptivity values were found to be 2.10 × 10(4) and 7.44 × 10(4) L mol(-1) cm(-1), for method B and method C, respectively.

摘要

描述了一种滴定法和两种分光光度法,这些方法简单、灵敏且经济,用于使用N-溴代琥珀酰亚胺(NBS)作为溴化剂测定原料药和片剂剂型中的琥珀酸舒马普坦(STS)。在滴定法中,将STS水溶液在乙酸介质中用计量过量的NBS处理,在判断STS溴化完全后,用碘量法测定未反应的NBS(方法A)。分光光度法包括在酸性介质中加入已知过量的NBS,然后通过其与过量碘化物的反应测定残留的NBS,释放出的碘(I3(-))要么在370nm处测量(方法B),要么释放出的碘与淀粉反应,然后在570nm处测量蓝色的淀粉-碘络合物(方法C)。滴定法适用于1.0-10.0mg STS范围(方法A),发现反应化学计量比为1:3(STS:NBS)。分光光度法在浓度范围0.6-15.0μg mL(-1)(方法B)和0.2-4.0μg mL(-1)(方法C)内符合比尔定律。方法B和方法C计算得到的表观摩尔吸光系数值分别为2.10×10(4)和7.44×10(4)L mol(-1)cm(-1)。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/73dd/3723360/282302c1d381/IJAC2013-934357.001.jpg

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