Spectrophotometric Determination of Penicillamine in Penicillamine Tablets
摘 要
青霉胺的巯基具有还原性,可将Fe(Ⅲ)还原Fe(Ⅱ),Fe(Ⅱ)能与2,2′-联吡啶形成桔红色的配合物,其最大吸收波长为524 nm,据此提出了分光光度法间接测定青霉胺药片中青霉胺含量的方法。优化的试验条件如下:① pH 4.5的0.2 mol·L-1乙酸-乙酸钠缓冲溶液用量为2.5 mL;② 0.2 g·L-1氯化铁溶液用量为2 mL;③ 1 g·L-1 2,2′-联吡啶溶液用量为2.5 mL;④ 显色时间为5 min。青霉胺的质量浓度在26 mg·L-1以内间接地与吸光度呈线性关系,检出限(3S/N)为0.01 mg·L-1。采用此法测定了青霉胺药片中青霉胺含量,所得测定值与标示量相符,测定值的相对标准偏差(n=5)为2.4%。
Abstract
Based on the reduction of Fe(Ⅲ) to Fe(Ⅱ) by penicillamine due to its sulfhydryl group and on the color reaction between the Fe(Ⅱ) ion and 2,2′-bipyridine to give a reddish orange colored complex with its absorption maximum at the wavelength of 524 nm, a spectrophotometric method for indirect determination of penicillamine in penicillamine tablets was proposed. The optimized conditions found were as follows: ① amount of 0.2 mol·L-1 HOAc-NaOAc buffer solution of pH 4.5: 2.5 mL; ② amount of 0.2 g·L-1 FeCl3 solution: 2 mL;③ amount of 1 g·L-1 2,2′-dipyridine solution: 2.5 mL; ④ time of reaction: 5 min. Linear relationship between values of absorbance and mass concentration of penicillamine was obtained (indirectly) in the range less than 26 mg·L-1, with detection limit (3S/N) of 0.01 mg·L-1. The proposed method was used in the analysis of penicillamine tablets, giving results of penicillamine contents in consistency with the labelled value with RSD (n=5) of 2.4%.
中图分类号 O657.32
所属栏目 工作简报
基金项目 广西教育厅项目(201103YB130);百色学院院级科研项目(2011KB03)
收稿日期 2012/12/17
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备注张金磊(1984-),女,山东聊城人,讲师,硕士,主要从事电化学分析和光度分析工作。
引用该论文: ZHANG Jin-lei,LAN Cui-ling,LI Hai-long,CAO Qing-hai. Spectrophotometric Determination of Penicillamine in Penicillamine Tablets[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(1): 40~42
张金磊,兰翠玲,李海龙,曹庆海. 分光光度法测定青霉胺药片中青霉胺含量[J]. 理化检验-化学分册, 2014, 50(1): 40~42
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参考文献
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【2】COROMINAS B G, PFERZSCHNER J, ICARDO M C, et al. In situ generation of Co(Ⅱ) by use of a solid-phase reactor in an FIA assembly for the spectrophotometric determination of penicillamine[J]. Journal of Pharmaceutical and Biomedical Analysis, 2005,39(1/2):281-284.
【3】何敏,赵书林,陈洁.青霉胺对映体的毛细管电泳手性分离及应用研究[J].分析化学, 2006,34(5):655-658.
【4】AMARNATH K, AMARNATH V, AMARNATH K, et al. A specific HPLC-UV method for the determination of cysteine and related aminothiols in biological samples[J]. Talanta, 2003,60(6):1229-1238.
【5】YAMASHITA G T, RABENSTEIN D L. Determination of penicillamine, penicillamine disulfide and penicillamine-glutathione mixed disulfide by high-performance liquid chromatography with electrochemical detection[J]. Journal of Chromatography B: Biomedical Sciences and Applications, 1989,491:341-354.
【6】袁玉,吴建平,宋建健,等.阻抑催化动力学法测定青霉胺[J].分析试验室, 2006,25(5):49-52.
【7】杨吉元,申爱卓,杜黎明,等.以黄连素/葫芦脲包合物为荧光探针测定青霉胺[J].分析化学, 2010,38(12):1813-1816.
【8】胡庆红,刘绍璞,罗红群.偶氮羧Ⅰ分光光度法测定蛋白质[J].分析科学学报, 2002,18(2):115-119.
【9】黄春芳,倪永年.分光光度法测定食品中的单宁[J].南昌大学学报:理科版, 2002,26(3):243-246.
【10】康春莉,郭平,李军,等.分光光度法测定硝普钠注射液中硝普钠的含量[J].吉林大学学报:理学版, 2003,41(3):402-405.
【11】SIANGPROH W, WANGFUENGKANAGUL N, CHAILAPAKUL O. Electrochemical oxidation of tiopronin at diamond film electrodes and its determination by amperometric flow injection analysis[J]. Anal Chim Acta, 2003,499(1/2):183-189.
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