Khan Muhammad Naeem, Jan Muhammad Rasul, Shah Jasmin, Lee Sang Hak
Department of Chemistry, Kyungpook National University, Daegu, 702-701, South Korea; Institute of Chemical Sciences, University of Peshawar, Pakistan.
Luminescence. 2014 May;29(3):266-74. doi: 10.1002/bio.2539. Epub 2013 Jun 11.
A simple and sensitive chemiluminescence (CL) method was developed for the determination of citalopram in pharmaceutical preparations and human plasma. The method is based on the enhancement of the weak CL signal of the luminol-H2 O2 system. It was found that the CL signal arising from the reaction between alkaline luminol and H2 O2 was greatly increased by the addition of silver nanoparticles in the presence of citalopram. Prepared silver nanoparticles (AgNPs) were characterized by UV-visible spectroscopy and transmission electron microscopy (TEM). Various experimental parameters affecting CL intensity were studied and optimized for the determination of citalopram. Under optimized experimental conditions, CL intensity was found to be proportional to the concentration of citalopram in the range 40-2500 ng/mL, with a correlation coefficient of 0.9997. The limit of detection (LOD) and limit of quantification (LOQ) of the devised method were 3.78 and 12.62 ng/mL, respectively. Furthermore, the developed method was found to have excellent reproducibility with a relative standard deviation (RSD) of 3.65% (n = 7). Potential interference by common excipients was also studied. The method was validated statistically using recovery studies and was successfully applied to the determination of citalopram in the pure form, in pharmaceutical preparations and in spiked human plasma samples. Percentage recoveries were found to range from 97.71 to 101.99% for the pure form, from 97.84 to 102.78% for pharmaceutical preparations and from 95.65 to 100.35% for spiked human plasma.
建立了一种简单灵敏的化学发光（CL）方法，用于测定药物制剂和人血浆中的西酞普兰。该方法基于鲁米诺-H2O2体系微弱CL信号的增强。研究发现，在西酞普兰存在下，加入银纳米颗粒可使碱性鲁米诺与H2O2反应产生的CL信号大幅增强。采用紫外可见光谱和透射电子显微镜（TEM）对制备的银纳米颗粒（AgNPs）进行了表征。研究并优化了影响CL强度的各种实验参数，用于西酞普兰的测定。在优化的实验条件下，发现CL强度与西酞普兰浓度在40-2500 ng/mL范围内成正比，相关系数为0.9997。所设计方法的检测限（LOD）和定量限（LOQ）分别为3.78和12.62 ng/mL。此外，所建立的方法具有出色的重现性，相对标准偏差（RSD）为3.65%（n = 7）。还研究了常见辅料的潜在干扰。通过回收率研究对该方法进行了统计学验证，并成功应用于纯品、药物制剂和加标人血浆样品中西酞普兰的测定。纯品的回收率为97.71%至101.99%，药物制剂为97.84%至102.78%，加标人血浆为95.65%至100.35%。
