School of Pharmacy, University of Oslo, PO Box 1068 Blindern, 0316 Oslo, Norway; G&T Septech AS, PO Box 33, 1917 Ytre Enebakk, Norway.
School of Pharmacy, University of Oslo, PO Box 1068 Blindern, 0316 Oslo, Norway.
J Chromatogr A. 2014 Jan 24;1326:7-12. doi: 10.1016/j.chroma.2013.12.028. Epub 2013 Dec 16.
In this work, a single-well electromembrane extraction (EME) device was developed based on a thin (100μm) and flat porous membrane of polypropylene supporting a liquid membrane. The new EME device was operated with a relatively large acceptor solution volume to promote a high recovery. Using this EME device, exhaustive extraction of the basic drugs quetiapine, citalopram, amitriptyline, methadone and sertraline was investigated from both acidified water samples and human plasma. The volume of acceptor solution, extraction time, and extraction voltage were found to be important factors for obtaining exhaustive extraction. 2-Nitrophenyl octyl ether was selected as the optimal organic solvent for the supported liquid membrane. From spiked acidified water samples (600μl), EME was carried out with 600μl of 20mM HCOOH as acceptor solution for 15min and with an extraction voltage of 250V. Under these conditions, extraction recoveries were in the range 89-112%. From human plasma samples (600μl), EME was carried out with 600μl of 20mM HCOOH as acceptor solution for 30min and with an extraction voltage of 300V. Under these conditions, extraction recoveries were in the range of 83-105%. When combined with LC-MS, the new EME device provided linearity in the range 10-1000ng/ml for all analytes (R(2)>0.990). The repeatability at low (10ng/ml), medium (100ng/ml), and high (1000ng/ml) concentration level for all five analytes were less than 10% (RSD). The limits of quantification (S/N=10) were found to be in the range 0.7-6.4ng/ml.
在这项工作中，开发了一种基于薄（100μm）且扁平的聚丙烯支撑液膜的单孔电膜萃取（EME）装置。新型 EME 装置采用相对较大的接受溶液体积进行操作，以促进高回收率。使用这种 EME 装置，从酸化水样和人血浆中研究了基本药物喹硫平、西酞普兰、阿米替林、美沙酮和舍曲林的完全萃取。发现接受溶液体积、萃取时间和萃取电压是获得完全萃取的重要因素。选择 2-硝基苯辛醚作为支撑液膜的最佳有机溶剂。从加标酸化水样（600μl）中，以 600μl 20mM HCOOH 作为接受溶液，在 15min 内进行 EME，并施加 250V 萃取电压。在这些条件下，萃取回收率在 89-112%范围内。从人血浆样品（600μl）中，以 600μl 20mM HCOOH 作为接受溶液，在 30min 内进行 EME，并施加 300V 萃取电压。在这些条件下，萃取回收率在 83-105%范围内。与 LC-MS 结合使用时，新型 EME 装置为所有分析物提供了 10-1000ng/ml 范围内的线性（R(2)>0.990）。所有五种分析物在低（10ng/ml）、中（100ng/ml）和高（1000ng/ml）浓度水平下的重复性均小于 10%（RSD）。定量限（S/N=10）在 0.7-6.4ng/ml 范围内。
