Hosseini Mehdi
Department of Chemistry, Faculty of Basic Sciences, Ayatollah Boroujerdi University, Boroujerd, Iran.
Anal Methods. 2024 Dec 12;16(48):8457-8470. doi: 10.1039/d4ay01668h.
A high-performance ionic liquid-based microextraction technique utilizing a task-specific imidazolium-based ionic liquid was employed for the analysis of paroxetine as a pharmaceutical pollutant at trace levels in some real environmental and biological samples. An ionic liquid, 3-(2-hydroxy-4-(isopropylamino)butyl)-1-methylimidazolium chloride, abbreviated to [Hibmim][Cl], was synthesized with a yield of 90.4%. Its physical properties were determined and characterized using FTIR, HNMR, CNMR, and CHNO techniques. The ionic liquid was then used for preconcentration prior to the determination of paroxetine in water and urine samples. Specifically, the ionic liquid served as both the extractor and the extracting phase, demonstrating high efficiency in extracting paroxetine from real samples. Density functional theory (DFT) studies, as well as UV-Vis and FTIR analyses indicated that the ionic liquid could successfully form a chelate with paroxetine hydrogen bonds. To confirm the method efficacy for analyzing real samples, the figures of merit and parameters affecting the microextraction procedure were assessed and optimized. Under optimal conditions, the limit of detection, limit of quantification, linear dynamic range, intra-day and inter-day relative standard deviations, preconcentration factor, and enhancement/enrichment factor were determined to be 0.42 μg L, 1.41 μg L, 5.0-60.0 μg L, 2.58%, 3.83%, 197.3, and 193.3, respectively. The maximum yield of paroxetine extraction under optimal conditions was 98.8%. Finally, to evaluate the method validity, a standard addition procedure was used, yielding satisfactory recovery values ranging from 98.7% to 101.2%.
一种基于高性能离子液体的微萃取技术，利用特定任务的咪唑基离子液体，用于分析一些实际环境和生物样品中痕量水平的帕罗西汀这种药物污染物。合成了一种离子液体3-(2-羟基-4-(异丙基氨基)丁基)-1-甲基咪唑氯化物，简称为[Hibmim][Cl]，产率为90.4%。使用傅里叶变换红外光谱(FTIR)、核磁共振氢谱(HNMR)、核磁共振碳谱(CNMR)和元素分析(CHNO)技术测定并表征了其物理性质。然后将该离子液体用于水和尿液样品中帕罗西汀测定前的预浓缩。具体而言，该离子液体既作为萃取剂又作为萃取相，在从实际样品中萃取帕罗西汀方面显示出高效率。密度泛函理论(DFT)研究以及紫外可见光谱(UV-Vis)和傅里叶变换红外光谱(FTIR)分析表明，该离子液体能够与帕罗西汀成功形成氢键螯合物。为了确认该方法分析实际样品的有效性，评估并优化了微萃取过程的品质因数和影响参数。在最佳条件下，检测限、定量限、线性动态范围、日内和日间相对标准偏差、预浓缩因子以及增强/富集因子分别确定为0.42 μg/L、1.41 μg/L、5.0 - 60.0 μg/L、2.58%、3.83%、197.3和193.3。在最佳条件下帕罗西汀萃取的最大产率为98.8%。最后，为了评估该方法的有效性，采用了标准加入法，回收率令人满意，范围为98.7%至101.2%。
