Suliman Fakhr Eldin O, Al-Lawati Zahra H, Al-Kindy Salma M Z
Department of Chemistry, College of Science, Sultan Qaboos University, Box 36, Al-Khod, 123, Sultanate of Oman.
J Fluoresc. 2008 Nov;18(6):1131-8. doi: 10.1007/s10895-008-0363-9. Epub 2008 May 22.
A simple, robust and sensitive sequential injection spectrofluorimetric method for the determination of penicillamine (PA) in pharmaceutical formulations is developed. The method is based on the formation of a highly fluorescent derivative when penicillamine is reacted with fluorescamine (FL) in borate buffer of pH 9.3. The derivative produced is monitored at an emission wavelength of 495 nm using an excitation wavelength of 355 nm. The optimum conditions for the determination of PA with FL were: 3 mM FL, pH 9.3, 5 mM methyl-beta-cyclodextrin, sample volume of 75 microL and reagent volume of 75 microL. Furthermore, the effect of various media on the fluorescence intensity of the PA-FL derivative was studied and methyl-beta-cyclodextrin was found to give the largest enhancement. A linear dynamic range for the determination of PA of 5-80 ppm was obtained with a sampling frequency of 50 h(-1) and a relative standard deviation of less than 2.5%. The method was applied to the determination of PA in pharmaceutical formulations with reasonable recoveries ranging from 101.0-103.1%, indicating that no interference is observed from concomitants usually present in dosage forms.
建立了一种用于测定药物制剂中青霉胺（PA）的简单、稳健且灵敏的顺序注射荧光光谱法。该方法基于青霉胺在pH 9.3的硼酸盐缓冲液中与荧光胺（FL）反应形成高荧光衍生物。使用355 nm的激发波长，在495 nm的发射波长下监测产生的衍生物。用FL测定PA的最佳条件为：3 mM FL、pH 9.3、5 mM甲基-β-环糊精、75 μL的样品体积和75 μL的试剂体积。此外，研究了各种介质对PA-FL衍生物荧光强度的影响，发现甲基-β-环糊精的增强作用最大。在50 h⁻¹的采样频率下，测定PA的线性动态范围为5-80 ppm，相对标准偏差小于2.5%。该方法应用于药物制剂中PA的测定，回收率合理，范围为101.0-103.1%，表明未观察到剂型中通常存在的共存物的干扰。
