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

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.

Effect of Selected Anionic and Cationic Drugs Affecting the Central Nervous System on Electrical Properties of Phosphatidylcholine Liposomes: Experiment and Theory

“…We choose the anionic barbituric acid because it is a compound of high pharmacological importance. However, there are a lack of studies concerning barbituric acid interactions with membrane components; only data for barbiturates, such as phenobarbital or pentobarbital, can be found [ 30 ].…”

Versatile Integration of Liquid-Phase Microextraction and Fluorescent Aptamer Beacons: A Synergistic Effect for Bioanalysis

“…26 In this process, the low-level target in biological samples can be preconcentrated in the simple acceptor solution, making it a promising technique for future integration with FABs. So far, several miniaturized membranebased LPME setups including in-vial LPME, 27 solvent bar LPME, 28 hollow-fiber LPME, 29 and flat membrane-based LPME (FM-LPME) 30 have been developed. Among these setups, FM-LPME attracted great attention due to its facile and convenient manipulation.…”

“…Among these setups, FM-LPME attracted great attention due to its facile and convenient manipulation. 30 Specifically, target extraction was achieved based on a wide-end sealed pipette tip. Hence, this miniaturized device will be selected for purification of the biological sample in the present work.…”

“…First, the miniaturized FM-LPME setup was fabricated according to the protocol in our recent work. 30 The FM-LPME setup was composed of three continuous phases including an acceptor phase, a SLM, and a donor phase. The acceptor phase house was a wide-end closed pipette tip sealed with a piece of flat polypropylene (PP) membrane.…”

“…So far, several miniaturized membrane-based LPME setups including in-vial LPME, solvent bar LPME, hollow-fiber LPME, and flat membrane-based LPME (FM-LPME) have been developed. Among these setups, FM-LPME attracted great attention due to its facile and convenient manipulation . Specifically, target extraction was achieved based on a wide-end sealed pipette tip.…”