Department of Analytical Chemistry and Pollutants, Shahid Beheshti University, G. C., P.O. Box 19396-4716, Evin, Tehran, Iran.
Department of Analytical Chemistry and Pollutants, Shahid Beheshti University, G. C., P.O. Box 19396-4716, Evin, Tehran, Iran.
J Pharm Biomed Anal. 2021 Feb 20;195:113862. doi: 10.1016/j.jpba.2020.113862. Epub 2020 Dec 23.
In this study, a new mode of gel electromembrane extraction (G-EME) namely as "Two-phase G-EME", is suggested for the sensitive quantification of five basic drugs (desipramine, clomipramine, trimipramine, citalopram and clozapine) in biological samples. Compared to classical G-EME which is based on aqueous-gel-aqueous layout, herein, the aqueous acceptor phase (AP) was replaced with organic solvent. Briefly, negative electrode was immersed into the organic AP (with low conductivity) and positive electrode into the aqueous donor phase (DP). Based on our results, this simple adjustment significantly reduced electroendosmosis (EEO) flow phenomenon which is considered as the main issue in G-EME. In the workflow, target analytes were extracted from the 7.0 mL sample, across the fabricated agarose gel membrane, to the 100 μL of the AP under the optimized extraction conditions (organic solvent type: acetonitrile; pH of gel membrane: 5.0, pH of sample solution: 4.0, voltage: 45 V and extraction time: 22 min). Then, the organic AP with analytes was analyzed by gas chromatography (GC) instrument with flame-ionization detector (FID). The methodology offered limits of detection (LODs) and recoveries in the range of 1.0-1.5 ng mL and 48.5-89.0 %, respectively. Finally, we note that two-phase G-EME assembly was able to extract analytes-of-interest in the convenient and safe manner from the hazardous and difficult-to-process biological specimens such as human serum and urine.
在这项研究中,提出了一种新的凝胶电迁移萃取模式(G-EME),即“两相 G-EME”,用于生物样品中五种基本药物(去甲丙咪嗪、氯米帕明、三甲丙咪嗪、西酞普兰和氯氮平)的灵敏定量。与基于水-凝胶-水布局的经典 G-EME 相比,本文用有机溶剂替代了水接受相(AP)。简而言之,负极浸入低电导率的有机溶剂 AP 中,正极浸入水供相(DP)中。根据我们的结果,这种简单的调整显著减少了电渗流(EEO)流动现象,这被认为是 G-EME 中的主要问题。在工作流程中,目标分析物从 7.0 mL 样品中提取,穿过制备的琼脂糖凝胶膜,在优化的提取条件下(有机溶剂类型:乙腈;凝胶膜 pH 值:5.0,样品溶液 pH 值:4.0,电压:45 V 和提取时间:22 分钟)进入 100 μL 的 AP 中。然后,用气相色谱仪(GC)和火焰离子化检测器(FID)分析含分析物的有机 AP。该方法的检测限(LOD)和回收率范围分别为 1.0-1.5 ng mL 和 48.5-89.0%。最后,我们注意到两相 G-EME 组件能够以方便和安全的方式从具有危害性和难以处理的生物标本(如人血清和尿液)中提取感兴趣的分析物。