In the present work, dispersive liquid-liquid microextraction (DLLME) was used to extract six synthetic cannabinoids (JWH-018, JWH-019, JWH-073, JWH-200, or WIN 55,225, JWH-250, and AM-694) from oral fluids. A rapid baseline separation of the analytes was achieved on a bidentate octadecyl silica hydride phase (Cogent Bidentate C18; 4.6 mm × 250 mm, 4 μm) maintained at 37 °C, by eluting in isocratic conditions (water:acetonitrile (25:75, V/V)). Detection was performed using positive electrospray ionization–tandem mass spectrometry. The parameters affecting DLLME (pH and ionic strength of the aqueous phase, type and volume of the extractant and dispersive solvent, vortex and centrifugation time) were optimized for maximizing yields. In particular, using 0.5 mL of oral fluid, acetonitrile (1 mL), was identified as the best option, both as a solvent to precipitate proteins and as a dispersing solvent in the DLLME procedure. To select an extraction solvent, a low transition temperature mixture (LTTM; composed of sesamol and chlorine chloride with a molar ratio of 1:3) and dichloromethane were compared; the latter (100 μL) was proved to be a better extractant, with recoveries ranging from 73 to 101 % by vortexing for 2 min. The method was validated according to the guidelines of Food and Drug Administration bioanalytical methods: within-run and between-run precisions ranged between 4 % and 18 % depending on the spike level and analyte; limits of detection spanned from 2 to 18 ng/mL; matrix-matched calibration curves were characterized by determination coefficients greater than 0.9914. Finally, the extraction procedure was compared with previous methods and with innovative techniques, presenting superior reliability, rapidity, simplicity, inexpensiveness, and efficiency.

Dispersive liquid-liquid microextraction, an effective tool for the determination of synthetic cannabinoids in oral fluid by liquid chromatography–tandem mass spectrometry / Tomai, P.; Gentili, A.; Curini, R.; Gottardo, R.; Franco, Tagliaro; Fanali, S.. - In: JOURNAL OF PHARMACEUTICAL ANALYSIS. - ISSN 2095-1779. - 11:3(2021), pp. 292-298. [10.1016/j.jpha.2020.11.004]

Dispersive liquid-liquid microextraction, an effective tool for the determination of synthetic cannabinoids in oral fluid by liquid chromatography–tandem mass spectrometry

Tomai P.
Primo
Validation
;
Gentili A.
Writing – Review & Editing
;
Curini R.
Writing – Original Draft Preparation
;
2021

Abstract

In the present work, dispersive liquid-liquid microextraction (DLLME) was used to extract six synthetic cannabinoids (JWH-018, JWH-019, JWH-073, JWH-200, or WIN 55,225, JWH-250, and AM-694) from oral fluids. A rapid baseline separation of the analytes was achieved on a bidentate octadecyl silica hydride phase (Cogent Bidentate C18; 4.6 mm × 250 mm, 4 μm) maintained at 37 °C, by eluting in isocratic conditions (water:acetonitrile (25:75, V/V)). Detection was performed using positive electrospray ionization–tandem mass spectrometry. The parameters affecting DLLME (pH and ionic strength of the aqueous phase, type and volume of the extractant and dispersive solvent, vortex and centrifugation time) were optimized for maximizing yields. In particular, using 0.5 mL of oral fluid, acetonitrile (1 mL), was identified as the best option, both as a solvent to precipitate proteins and as a dispersing solvent in the DLLME procedure. To select an extraction solvent, a low transition temperature mixture (LTTM; composed of sesamol and chlorine chloride with a molar ratio of 1:3) and dichloromethane were compared; the latter (100 μL) was proved to be a better extractant, with recoveries ranging from 73 to 101 % by vortexing for 2 min. The method was validated according to the guidelines of Food and Drug Administration bioanalytical methods: within-run and between-run precisions ranged between 4 % and 18 % depending on the spike level and analyte; limits of detection spanned from 2 to 18 ng/mL; matrix-matched calibration curves were characterized by determination coefficients greater than 0.9914. Finally, the extraction procedure was compared with previous methods and with innovative techniques, presenting superior reliability, rapidity, simplicity, inexpensiveness, and efficiency.
2021
dispersive liquid-liquid microextraction; Illicit drugs; microextraction techniques; silica C-based column; synthetic cannabinoids
01 Pubblicazione su rivista::01a Articolo in rivista
Dispersive liquid-liquid microextraction, an effective tool for the determination of synthetic cannabinoids in oral fluid by liquid chromatography–tandem mass spectrometry / Tomai, P.; Gentili, A.; Curini, R.; Gottardo, R.; Franco, Tagliaro; Fanali, S.. - In: JOURNAL OF PHARMACEUTICAL ANALYSIS. - ISSN 2095-1779. - 11:3(2021), pp. 292-298. [10.1016/j.jpha.2020.11.004]
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11573/1576666
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