Instituto de Química Rosario (CONICET-UNR), Facultad de Ciencias Bioquímicas y Farmacéuticas, Universidad Nacional de Rosario, Suipacha 531, 2000 Rosario, Argentina.
Talanta. 2010 Jun 30;82(1):325-32. doi: 10.1016/j.talanta.2010.04.043. Epub 2010 Apr 24.
The present article describes the spectrofluorimetric determination of galantamine, a widely used acetylcholinesterase inhibitor, through excitation-emission fluorescence matrices and second-order calibration. With the purpose of enhancing the fluorescence intensity of this substance, the effect of different organized assemblies was evaluated. Although the interaction of galantamine with different cyclodextrins is weak, it was corroborated that the fluorescence intensity of this pharmaceutical in the presence of alpha-cyclodextrin is increased by a twofold factor. Among the studied micellar media, the anionic surfactant sodium dodecyl sulfate produced the largest signals for the compound of interest (sixfold enhancement), and was selected as auxiliary reagent for the subsequent determinations. The developed approach enabled the determination of galantamine at the ng mL(-1) level without the necessity of applying separation steps, and in the presence of uncalibrated interferences. The applied second-order chemometric tools were parallel factor analysis (PARAFAC), unfolded partial least-squares coupled to residual bilinearization (U-PLS/RBL), and multidimensional partial least-squares coupled to residual bilinearization (N-PLS/RBL). The ability of U-PLS/RBL to successfully overcome spectral interference problems is demonstrated. The quality of the proposed method was established with the determination of galantamine in both artificial and natural water samples.
本文描述了通过激发-发射荧光矩阵和二阶校准来测定加兰他敏的分光荧光法。为了增强该物质的荧光强度,评估了不同有序组装的效果。虽然加兰他敏与不同环糊精的相互作用较弱,但证实了在α-环糊精存在下,该药物的荧光强度增强了一倍。在所研究的胶束介质中,阴离子表面活性剂十二烷基硫酸钠使目标化合物(六倍增强)产生了最大信号,并被选为后续测定的辅助试剂。该方法不需要采用分离步骤,在存在未校准干扰的情况下,可在纳克/毫升(ng/mL)水平测定加兰他敏。所应用的二阶化学计量学工具包括平行因子分析(PARAFAC)、解卷偏最小二乘与残差双线性化(U-PLS/RBL)和多维偏最小二乘与残差双线性化(N-PLS/RBL)。证明了 U-PLS/RBL 成功克服光谱干扰问题的能力。通过在人工和天然水样中测定加兰他敏,确定了所提出方法的质量。