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电辅助溶剂搅拌棒微萃取-高效液相色谱法用于生物样品中碱性药物的提取与定量分析。

Development of electrically assisted solvent bar microextraction followed by high performance liquid chromatography for the extraction and quantification of basic drugs in biological samples.

机构信息

Department of Analytical Chemistry and Pollutants, Shahid Beheshti University, G. C., Evin, Tehran 1983963113, Iran.

Department of Analytical Chemistry and Pollutants, Shahid Beheshti University, G. C., Evin, Tehran 1983963113, Iran.

出版信息

J Chromatogr A. 2021 Sep 27;1654:462447. doi: 10.1016/j.chroma.2021.462447. Epub 2021 Aug 5.

DOI:10.1016/j.chroma.2021.462447
PMID:34392124
Abstract

In this study, a new extraction procedure is introduced based on electrically assisted solvent bar microextraction. In the first step, the analytes are transferred from sample solution to the hollow fiber supported organic solvent. After that, with the aid of an electrical field, the analytes migrated into the aqueous extractant. The proposed approach was used to extract the three basic drugs (including lidocaine, diltiazem, and propranolol) from the plasma and urine samples. Under the optimized condition, (the supported organic solvent: 1-octanol, stirring rate: 300 rpm, pH of sample solution: 12.0, salt concentration: 2.0% (w/v), extraction time: 15 min, aqueous extractant: (30 µL, 100 mM HCl), back-extraction time: 2 min, back-extraction voltage: 100 V), the proposed procedure presented wide linearities with coefficients of determination more than 0.992 over a concentration range of 5.0-1000 ng mL. The limit of detection was also determined in the range of 0.5 to 5.0 ng mL, repeatability (intra-day) was between 3.3 and 11.1% (n = 4), and reproducibility (inter-day) was between 4.3 and 14.6% (n = 4 days). It was indicated that the proposed approach could effectively extract the analytes from the plasma and urine samples, and the relative recoveries were between 90.2 and 105.6%, indicating the validity of this method.

摘要

在本研究中,提出了一种基于电场辅助溶剂支撑膜微萃取的新萃取方法。在第一步中,分析物从样品溶液转移到中空纤维支撑的有机溶剂中。之后,在电场的辅助下,分析物迁移到水相萃取剂中。该方法用于从血浆和尿液样品中提取三种碱性药物(包括利多卡因、地尔硫卓和普萘洛尔)。在优化条件下(支撑有机溶剂:1-辛醇,搅拌速度:300 rpm,样品溶液 pH 值:12.0,盐浓度:2.0%(w/v),萃取时间:15 min,水相萃取剂:(30 µL,100 mM HCl),反萃取时间:2 min,反萃取电压:100 V),该方法在 5.0-1000 ng mL 的浓度范围内呈现出宽的线性,相关系数均大于 0.992。检测限也在 0.5 至 5.0 ng mL 的范围内确定,重复性(日内)在 3.3%至 11.1%(n=4)之间,重现性(日间)在 4.3%至 14.6%(n=4 天)之间。结果表明,该方法可以有效地从血浆和尿液样品中提取分析物,相对回收率在 90.2%至 105.6%之间,表明该方法有效。

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