高选择性灵敏荧光光谱法测定药品和生物液中n -乙酰-4-氨基酚(IV)

IF 0.4 Q4 CHEMISTRY, ANALYTICAL
M. J. Ahmed
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引用次数: 2

摘要

建立了一种简单、快速、超灵敏、高选择性、非萃取的超痕量n-乙酰-4-氨基酚(扑热息痛)的荧光光谱测定方法。本方法以对乙酰氨基酚在微酸性(0.05 ~ 0.15 M H2SO4)水溶液中氧化为基础,用提示氧化剂铈(IV)对乙酰氨基酚进行了直接荧光光谱测定,荧光物质是对乙酰氨基酚的氧化产物,激发波长为λex = 255 nm,发射波长为λem = 350 nm。氧化产物的荧光强度在15分钟内达到恒定值(在45±5℃加热5分钟后),并在24小时以上保持稳定。对影响反应条件的众多变量,如铈(IV)的浓度、温度、酸度的影响、反应时间和溶剂进行了谨慎的实验和优化。对乙酰氨基酚的检出限为2μgL-1,得到10 ~ 700μ gl -1的线性校准图;反应体系的定量限为10μgL-1;RSD为0 ~ 2%,相关系数R2 = 0.9999。在100μgL-1水平对乙酰氨基酚的测定中,检测了40多种常见的剂型中存在的潜在干扰辅料,不干扰测定过程。该方法已成功地应用于商业制剂和生物液中扑热息痛的含量测定。所提出的药物和生物分析方法的结果与分光光度法和英国药典中规定的官方方法相似,并被发现在一个很好的一致性。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
A Highly Selective and Sensitive Spectrofluorimetric Method for the Determination of N-acetyl-4-aminophenol at Nano-trace Levels in Pharmaceuticals and Biological Fluids Using Cerium (IV)
A very simple, rapid, ultra-sensitive, highly selective and non-extractive spectrofluorimetric method for the determination of N-acetyl-4-aminophenol (paracetamol) at ultra-trace levels has been developed. This method was based on the oxidation of paracetamol in presence of slightly acidic (0.05 – 0.15 M H2SO4) aqueous solution with a prompt oxidizing agent, cerium(IV) for the direct spectrofluorimetric determination of paracetamol and the fluorescent species is an oxidation product of parcetamol, has excitation and emission wavelength at λex = 255 nm and λem = 350 nm, respectively. The fluorescence intensity of oxidation product reaches a constant value (after heating for 5 min at 45 ± 5°C) within 15 min remains stable for over 24 h. Numerous variables influencing the reaction’s conditions e.g. the concentrations of cerium(IV), temperature, effect of acidity, time of the reaction and solvents were cautiously experimented and optimized. Linear calibration graphs were obtained for 10–700μgL-1 of paracetamol, having a detection limit of 2μgL-1; the quantification limit of the reaction system was found to be 10μgL-1; the RSD was 0 – 2 % and the correlation coefficient, R2 = 0.9999. A large excess of over 40 potentially interfering excipients, commonly present in dosage forms were tested in the determination of paracetamol at 100μgL-1 level, do not intervene in the determination process. The developed method was successfully applied to the determination of paracetamol in commercial pharmaceutical formulations and biological fluids. The results of the proposed method for pharmaceuticals and biological analyses were analogous with that of spectrophotometric method and the Official method stated in the British Pharmacopoeia, and was found to be in an excellent agreement.
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来源期刊
CiteScore
1.10
自引率
16.70%
发文量
16
审稿时长
15 weeks
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