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零角度荧光分光光度法:乙酰水杨酸药物制剂中水杨酸的测定

Spectrofluorimetry at zero angle: determination of salicylic acid in an acetylsalicylic acid pharmaceutical formulation.

作者信息

Villari A, Micali N, Fresta M, Puglisi G

机构信息

Dipartimento Farmaco-Chimico Università di Messina, Italy.

出版信息

Analyst. 1994 Jul;119(7):1561-5. doi: 10.1039/an9941901561.

Abstract

In this work, a solid-state spectrofluorimetric method for drug assays was developed. In particular, we report the determination of salicylic acid (SA), as a hydrolysis product, in solid pharmaceutical formulations containing acetylsalicylic acid (ASA). Recently, we described a sensitive and accurate fluorescence method that provided, through a mathematical application, the simultaneous determination of ASA and SA. By means of the spectrofluorimetric method reported herein it was possible to carry out the SA determination, without any mathematical calculation and with a sensitivity 100 times that of our previous method. The intra- and inter-day reproducibility of the spectrofluorimetric method, expressed as the relative standard deviation, ranged from 0.1 to 0.3%. The present method requires a fluorescence apparatus with the excitation and detection systems in-line (zero angle). The detection system was not sensitive to the excitation wavelength, but was highly sensitive to emission wavelengths from 350 to 800 nm. The results obtained were compared with those of our previous spectrofluorimetric method, together with those of a high-performance liquid chromatography method and a US Pharmacopeia method. The sensitivity of the method was of the order of 10(-8) g.

摘要

在本研究中,开发了一种用于药物分析的固态荧光光谱法。具体而言,我们报告了在含有乙酰水杨酸(ASA)的固体药物制剂中,作为水解产物的水杨酸(SA)的测定方法。最近,我们描述了一种灵敏且准确的荧光方法,该方法通过数学应用能够同时测定ASA和SA。通过本文报道的荧光光谱法,可以在无需任何数学计算的情况下进行SA的测定,并且灵敏度是我们之前方法的100倍。荧光光谱法的日内和日间重现性以相对标准偏差表示,范围为0.1%至0.3%。本方法需要一台激发和检测系统在线(零角度)的荧光仪器。检测系统对激发波长不敏感,但对350至800nm的发射波长高度敏感。将获得的结果与我们之前的荧光光谱法结果、高效液相色谱法结果以及美国药典方法的结果进行了比较。该方法的灵敏度约为10(-8) g。

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