Department of Analytical Chemistry, Universitat Autónoma de Barcelona, 08193, Bellaterra, Barcelona, Spain.
Department of Pharmacy, University of Oslo, P.O. Box 1068 Blindern, 0316, Oslo, Norway; Department of Pharmacy, Faculty of Health and Medical Sciences University of Copenhagen, Universitetesparken 2, 2100, Copenhagen Ø, Denmark.
Anal Chim Acta. 2022 May 22;1208:339829. doi: 10.1016/j.aca.2022.339829. Epub 2022 Apr 11.
In sample preparation, simultaneous extraction of analytes of very different polarity from biological matrixes represents a challenge. In this work, verapamil hydrochloride (VRP), amitriptyline (AMP), tyramine (TYR), atenolol (ATN), metopropol (MTP) and nortriptyline (NRP) were used as basic model analytes and simultaneously extracted from urine samples by liquid-phase microextraction (LPME) in a microfluidic device. The model analytes (target compounds) were pharmaceuticals with 0.4 < log P < 5. Different organic solvents and mixtures of them were investigated as supported liquid membrane (SLM), and a mixture of 2:1 (v/v) tributyl phosphate (TBP) and dihexyl ether (DHE) was found to be highly efficient for the simultaneous extraction of the non-polar and polar model analytes. TBP reduced the intrinsic hydrophobicity of the SLM and facilitated extraction of polar analytes, while DHE served to minimize trapping of non-polar analytes. Sample and acceptor phase composition were adjusted to pH 12 and pH 1.5, respectively. Urine samples were pumped into the microfluidic system at 1 μL min-1 and the extraction was completed in 7 min. Recoveries exceeded 78% for the target analytes, and the relative standard deviation (n = 4) was below 7% in all cases. Using five microliters of SLM, the microfluidic extraction system showed good long-term stability, and the same SLM was used for more than 18 consecutive extractions.
在样品制备中，从生物基质中同时提取非常不同极性的分析物是一个挑战。在这项工作中，盐酸维拉帕米（VRP）、阿米替林（AMP）、酪胺（TYR）、阿替洛尔（ATN）、美托洛尔（MTP）和去甲替林（NRP）被用作基本模型分析物，并通过微流控装置中的液相微萃取（LPME）从尿样中同时提取。模型分析物（目标化合物）是具有 0.4<log P<5 的药物。研究了不同的有机溶剂及其混合物作为支撑液膜（SLM），发现 2:1（v/v）磷酸三丁酯（TBP）和二己基醚（DHE）的混合物对非极性和极性模型分析物的同时萃取非常有效。TBP 降低了 SLM 的固有疏水性，有利于极性分析物的萃取，而 DHE 则有助于最小化非极性分析物的捕获。样品和接受相的组成分别调整至 pH 12 和 pH 1.5。尿样以 1μL min-1 的速度泵入微流控系统，萃取在 7 min 内完成。对于目标分析物，回收率超过 78%，在所有情况下，相对标准偏差（n=4）均低于 7%。使用 5 微升 SLM，微流控萃取系统表现出良好的长期稳定性，并且相同的 SLM 用于超过 18 次连续萃取。
