Department of Chemistry, Shahid Beheshti University, Tehran, Iran.
J Sep Sci. 2011 Jun;34(11):1275-82. doi: 10.1002/jssc.201000919. Epub 2011 Apr 13.
Ultrasound-assisted emulsification microextraction based on the solidification of floating organic droplet combined with high-performance liquid chromatography-ultra violet (HPLC-UV) detection was applied for the extraction and determination of fluoxetine, citalopram, and venlafaxine as antidepressants drugs in biological samples. In total, 30 μL of undecanol was injected slowly into a glass-centrifuge tube containing 5 mL alkaline sample solution that was located inside the ultrasonic water bath. The formed emulsion was centrifuged and the fine droplets of solvent were floated at the top of the test tube. The test tube was then cooled in an ice bath and the solidified solvent transferred into a conical vial; it melted quickly at room temperature. Then the analysis of the extracts was carried out by high-performance liquid chromatography. Under optimal conditions, the preconcentration factors were between 174 and 316. Detection limits (LODs) of 3 μg/L were obtained and the calibration graphs were linear within the range of 10-1000 μg/L. Finally, the feasibility of the proposed method was successfully confirmed by extraction and determination of the antidepressant drugs in human urine and plasma samples in the range of microgram per liter and suitable results were obtained.
基于固态浮油的超声辅助乳化微萃取结合高效液相色谱-紫外(HPLC-UV)检测法,用于萃取和测定生物样品中的氟西汀、西酞普兰和文拉法辛等抗抑郁药物。总共向装有 5 mL 碱性样品溶液的玻璃离心管中缓慢注入 30 μL 十一醇,该溶液位于超声水浴中。形成的乳状液经离心后,溶剂的细小液滴浮在试管顶部。然后将试管在冰浴中冷却,将凝固的溶剂转移到锥形小瓶中;它在室温下迅速融化。然后通过高效液相色谱法对提取物进行分析。在最佳条件下,预浓缩因子在 174 到 316 之间。检测限(LOD)为 3μg/L,校准曲线在 10-1000μg/L 范围内呈线性。最后,通过在微克/升范围内对人尿和血浆样品中的抗抑郁药物进行萃取和测定,成功验证了该方法的可行性,得到了令人满意的结果。