Bavili Tabrizi Ahad, Rezazadeh Ahmad
Department of Medicinal Chemistry, Faculty of Pharmacy and Biotechnology Research Center, Tabriz University of Medical Sciences, Tabriz, Iran.
Adv Pharm Bull. 2012;2(2):157-64. doi: 10.5681/apb.2012.024. Epub 2012 Jun 15.
Fluoxetine is the most prescribed antidepressant drug worldwide. In this work, a new dispersive liquid-liquid microextraction (DLLME) method combined with spectrofluorimetry has been developed for the extraction and determination of FLX in pharmaceutical formulations and human urine.
For FLX determination, the pH of a 10 mL of sample solution containing FLX, was adjusted to 11.0. Then, 800 µL of ethanol containing 100 µL of chloroform was injected rapidly into the sample solution. A cloudy solution was formed and FLX extracted into the fine droplets of chloroform. After centrifugation, the extraction solvent was sedimented and supernatant aqueous phase was readily decanted. The remained organic phase was diluted with ethanol and its fluorescence was measured at 292±3 nm after excitation at 234±3 nm.
Some important parameters influencing microextraction efficiency were investigated. Under the optimum extraction conditions, a linear calibration curve in the range of 10 to 800 ng/mL with a correlation coefficient of r(2) = 0.9993 was obtained. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 2.78 and 9.28 ng/mL, respectively. The relative standard deviations (RSDs) were less than 4%. Average recoveries for spiked samples were 93-104%.
The proposed method gives a very rapid, simple, sensitive, wide dynamic range and low-cost procedure for the determination of FLX.
氟西汀是全球处方量最大的抗抑郁药物。在本研究中，开发了一种新的分散液液微萃取（DLLME）方法并结合荧光光谱法，用于药物制剂和人尿中氟西汀的萃取和测定。
为测定氟西汀，将10 mL含氟西汀的样品溶液的pH值调至11.0。然后，将含有100 μL氯仿的800 μL乙醇迅速注入样品溶液中。形成浑浊溶液，氟西汀被萃取到氯仿微滴中。离心后，萃取溶剂沉淀，上清液水相易于倾析。剩余有机相用乙醇稀释，在234±3 nm激发后，于292±3 nm处测量其荧光。
研究了影响微萃取效率的一些重要参数。在最佳萃取条件下，获得了10至800 ng/mL范围内的线性校准曲线，相关系数r(2)=0.9993。检测限（LOD）和定量限（LOQ）分别为2.78和9.28 ng/mL。相对标准偏差（RSD）小于4%。加标样品的平均回收率为93 - 104%。
所提出的方法为氟西汀的测定提供了一种非常快速、简单、灵敏、动态范围宽且低成本的程序。
