Salinas-Castillo A, Carretero A Segura, Fernández-Gutiérrez A
Department of Analytical Chemistry, Faculty of Sciences, University of Granada, C/ Fuentenueva s/n, 18071 Granada, Spain.
Anal Bioanal Chem. 2003 Aug;376(7):1111-4. doi: 10.1007/s00216-003-2052-5. Epub 2003 Jun 27.
The applicability of heavy atom-induced room-temperature phosphorescence to pharmaceutical samples is demonstrated in this work. Thus a new, simple, rapid, and selective phosphorimetric method for dipyridamole determination is proposed. The phosphorescence signals are a consequence of intermolecular protection when analytes are exclusively in the presence of heavy atom salts and sodium sulfite as an oxygen scavenger to minimize RTP quenching. The determination was performed in 0.1 mol L(-1) thallium(I) nitrate and 8 mmol L(-1) sodium sulfite at a measurement temperature of 20 degrees C. The phosphorescence intensity was measured at 635 nm, with excitation at 305 nm. Phosphorescence was easily developed; a linear concentration range was obtained between 0 and 100 ng mL(-1) with a detection limit of 940 ng L(-1), an analytical sensitivity of 2.5 ng mL(-1), and a standard deviation of 2.7% at 60 ng mL(-1) concentration. The method has been successfully applied to the analysis of dipyridamole in a unique Spanish commercial formulation containing 100 ng mL(-1) per capsule. The recovery was 101.6% with 6.5% standard deviation of analytical measurement. The method using the standard addition methodology has been validated.
本工作证明了重原子诱导室温磷光在药物样品中的适用性。因此，提出了一种测定双嘧达莫的新的、简单、快速且选择性的磷光分析法。当分析物仅在重原子盐和作为氧清除剂的亚硫酸钠存在下时，磷光信号是分子间保护的结果，以最小化室温磷光猝灭。测定在0.1 mol L(-1)硝酸铊(I)和8 mmol L(-1)亚硫酸钠中于20℃的测量温度下进行。在635 nm处测量磷光强度，激发波长为305 nm。磷光易于产生；在0至100 ng mL(-1)之间获得线性浓度范围，检测限为940 ng L(-1)，分析灵敏度为2.5 ng mL(-1)，在60 ng mL(-1)浓度下标准偏差为2.7%。该方法已成功应用于一种独特的西班牙商业制剂中双嘧达莫的分析，该制剂每胶囊含100 ng mL(-1)。回收率为101.6%，分析测量的标准偏差为6.5%。使用标准加入法的该方法已得到验证。
