Application of a Low Transition Temperature Mixture for the Dispersive Liquid-Liquid Microextraction of Illicit Drugs from Urine Samples

The use of psychoactive substances is a serious problem in today's society and reliable methods of analysis are necessary to confirm their occurrence in biological matrices. In this work, a green sample preparation technique prior to HPLC-MS analysis was successfully applied to the extraction o...

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Bibliographic Details
Published in:Molecules (Basel, Switzerland) Switzerland), 2021-08, Vol.26 (17), p.5222
Main Authors: Gallo, Valeria, Tomai, Pierpaolo, Di Lisio, Valerio, Dal Bosco, Chiara, D'Angelo, Paola, Fanali, Chiara, D'Orazio, Giovanni, Silvestro, Ilaria, Picó, Yolanda, Gentili, Alessandra
Format: Article
Language:English
Subjects:
Amphetamines
Choline
Cocaine
Cold Temperature
deep eutectic solvents
Dispersion
dispersive liquid–liquid microextraction
Drugs
Ecstasy
Extraction procedures
Glass transition temperature
High-performance liquid chromatography
Humans
Hydrogen bonds
illicit drugs
Illicit Drugs - chemistry
Limit of Detection
Liquid chromatography
Liquid Phase Microextraction - methods
low transition temperature mixtures
Parameter estimation
Quantitation
Sample preparation
Solvents
Transition Temperature
Transition temperatures
Urine
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Summary:The use of psychoactive substances is a serious problem in today's society and reliable methods of analysis are necessary to confirm their occurrence in biological matrices. In this work, a green sample preparation technique prior to HPLC-MS analysis was successfully applied to the extraction of 14 illicit drugs from urine samples. The isolation procedure was a dispersive liquid-liquid microextraction based on the use of a low transition temperature mixture (LTTM), composed of choline chloride and sesamol in a molar ratio 1:3 as the extracting solvent. This mixture was classified as LTTM after a thorough investigation carried out by FTIR and DSC, which recorded a glass transition temperature at -71 °C. The extraction procedure was optimized and validated according to the main Food and Drug Administration (FDA) guidelines for bioanalytical methods, obtaining good figures of merit for all parameters: the estimated lower limit of quantitation (LLOQ) values were between 0.01 µg L (bk-MMBDB) and 0.37 µg L (PMA); recoveries, evaluated at very low spike levels (in the ng-µg L range), spanned from 55% (MBDB) to 100% (bk-MMBDB and MDPV); finally, both within-run and between-run precisions were lower than 20% (LLOQ) and 15% (10xLLOQ).
ISSN:1420-3049
1420-3049
DOI:10.3390/molecules26175222