Department of Chemistry, Kyungpook National University, Daegu 702-701, South Korea.
J Fluoresc. 2013 Jan;23(1):161-9. doi: 10.1007/s10895-012-1129-y. Epub 2012 Sep 27.
A simple, sensitive, and accurate spectrofluorimetric method was developed for the determination of citalopram in bulk and pharmaceutical preparations. The method is based on the enhancement of the weak fluorescence signal (FL) of the Tb (III)-citalopram system in the presence of silver nanoparticles. Fluorescence intensities were measured at 555 nm after excitation at 281 nm. Prepared silver nanoparticles (AgNPs) were characterized by UV-Visible spectra and transmission electron microscopy (TEM). Various factors affecting the formation of citalopram-Tb (III)-AgNPs complexes were studied and optimized. The fluorescence intensity versus concentration plot was linear over the range 0.02-14 μg mL(-1), with an excellent correlation coefficient of 0.9978. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 7.15 × 10(-6) μg mL(-1) and 2.38 × 10(-5) μg mL(-1) respectively. The proposed method was found to have good reproducibility with a relative standard deviation of 3.66% (n = 6). The interference effects of common excipients found in pharmaceutical preparations were studied. The developed method was validated statistically by performing recoveries studies and successfully applied for the assay of citalopram in bulk powder and pharmaceutical preparations. Percent recoveries were found to range from 98.98% to 100.97% for bulk powder and from 96.57% to 101.77% for pharmaceutical preparations.
建立了一种简单、灵敏、准确的荧光分光光度法，用于测定原料药和制剂中的西酞普兰。该方法基于在银纳米粒子存在下增强西酞普兰与铽（III）体系的弱荧光信号（FL）。在 281nm 激发下，在 555nm 处测量荧光强度。通过紫外-可见光谱和透射电子显微镜（TEM）对制备的银纳米粒子（AgNPs）进行了表征。研究并优化了影响西酞普兰-Tb（III）-AgNPs 配合物形成的各种因素。荧光强度与浓度的关系图在 0.02-14μgmL(-1)范围内呈线性，相关系数为 0.9978。检测限（LOD）和定量限（LOQ）分别为 7.15×10(-6)μgmL(-1)和 2.38×10(-5)μgmL(-1)。该方法具有良好的重现性，相对标准偏差为 3.66%（n=6）。研究了制剂中常见赋形剂的干扰影响。通过进行回收率研究对所提出的方法进行了统计学验证，并成功应用于原料药和制剂中西酞普兰的测定。原料药的回收率范围为 98.98%-100.97%，制剂的回收率范围为 96.57%-101.77%。
