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Determination of Barbiturates in Biological Specimens by Flat Membrane-Based Liquid-Phase Microextraction and Liquid Chromatography-Mass Spectrometry

Department of Forensic Medicine, Huazhong University of Science and Technology, 13 Hangkong Road, Wuhan 430030, China
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Author to whom correspondence should be addressed.
These authors contributed equally to this work.
Academic Editor: Nuno Neng
Molecules 2019, 24(8), 1494; https://doi.org/10.3390/molecules24081494
Received: 19 March 2019 / Revised: 9 April 2019 / Accepted: 16 April 2019 / Published: 16 April 2019
(This article belongs to the Special Issue Modern Sample Preparation Approaches for Separation Science)
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Abstract

The wide abuse of barbiturates has aroused extensive public concern. Therefore, the determination of such drugs is becoming essential in therapeutic drug monitoring and forensic science. Herein, a simple, efficient, and inexpensive sample preparation technique, namely, flat membrane-based liquid-phase microextraction (FM-LPME) followed by liquid chromatography-mass spectrometry (LC-MS), was used to determine barbiturates in biological specimens. Factors that may influence the efficiency including organic extraction solvent, pH, and composition of donor and acceptor phases, extraction time, and salt addition to the sample (donor phase) were investigated and optimized. Under the optimized extraction conditions, the linear ranges of the proposed FM-LPME/LC-MS method (with correlation coefficient factors ≥ 0.99) were 7.5–750 ng mL−1 for whole blood, 5.0–500 ng mL−1 for urine, and 25–2500 ng g−1 for liver. Repeatability between 5.0 and 13.7% was obtained and the limit of detection (LOD) values ranged from 1.5 to 3.1 ng mL−1, from 0.6 to 3.6 ng mL−1, and from 5.2 to 10.0 ng g−1 for whole blood, urine, and liver samples, respectively. This method was successfully applied for the analysis of barbiturates in blood and liver from rats treated with these drugs, and excellent sample cleanup was achieved. View Full-Text
Keywords: membrane-based microextraction; barbiturates; simultaneous determination; whole blood; urine; liver membrane-based microextraction; barbiturates; simultaneous determination; whole blood; urine; liver
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited (CC BY 4.0).
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Zhu, R.; Dong, Y.; Cai, X.; Huang, C. Determination of Barbiturates in Biological Specimens by Flat Membrane-Based Liquid-Phase Microextraction and Liquid Chromatography-Mass Spectrometry. Molecules 2019, 24, 1494.

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