Determination of Lysergic Acid Diethylamide and 2-Oxo-3-Hydroxy-LSD in Blood: Validation and Comparison of Two Liquid Chromatography–Tandem Mass Spectrometry Methods
Lysergic acid diethylamide (LSD) is a powerful hallucinogen. Its detection is limited by its low dosage; moreover, LSD is rapidly metabolized into 2-oxo-3-hydroxy-LSD (O-H-LSD). In this study we validated two methods for determination of LSD and O-H-LSD in blood. Method #1 consisted in the upgrade o...
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MDPI AG
2023-09-01
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| author | Alexandra Dimitrova Maria Grazia Di Milia Regina Rensi Simone Grassi Barbara Gualco Fabio Vaiano |
| author_facet | Alexandra Dimitrova Maria Grazia Di Milia Regina Rensi Simone Grassi Barbara Gualco Fabio Vaiano |
| author_sort | Alexandra Dimitrova |
| collection | DOAJ |
| description | Lysergic acid diethylamide (LSD) is a powerful hallucinogen. Its detection is limited by its low dosage; moreover, LSD is rapidly metabolized into 2-oxo-3-hydroxy-LSD (O-H-LSD). In this study we validated two methods for determination of LSD and O-H-LSD in blood. Method #1 consisted in the upgrade of a previously developed procedure for detection of 163 compounds. Method #2 was specific for LSD and O-H-LSD. Analyses were performed through LC-MS/MS by dynamic (#1) and/or MRM mode (#2), in positive ionization. Transitions were: 324→223,208 <i>m</i>/<i>z</i> for LSD; 356→237,222 <i>m</i>/<i>z</i> for O-H-LSD. Validations were performed following the AAFS’s guidelines. Linearity was good for both methods. Sensitivity was in line with previously validated methods with LOQs at 0.0375 (#1) and 0.025 (#2) ng/mL for LSD and 0.01875 (#1) and 0.0125 (#2) ng/mL for O-H-LSD. Bias and %CV always met the acceptance criteria. RRs were >83%, except for O-H-LSD with method #1. The methods were successfully applied to two real cases. Method #1 proved to be useful for screening purposes, while method #2 can represent a sensitive and reliable tool for confirmation procedures. |
| first_indexed | 2024-03-10T22:00:24Z |
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| institution | Directory Open Access Journal |
| issn | 2297-8739 |
| language | English |
| last_indexed | 2024-03-10T22:00:24Z |
| publishDate | 2023-09-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Separations |
| spelling | doaj.art-5d3bd5071d2e4cf38995cf454c89c3482023-11-19T12:58:03ZengMDPI AGSeparations2297-87392023-09-0110950210.3390/separations10090502Determination of Lysergic Acid Diethylamide and 2-Oxo-3-Hydroxy-LSD in Blood: Validation and Comparison of Two Liquid Chromatography–Tandem Mass Spectrometry MethodsAlexandra Dimitrova0Maria Grazia Di Milia1Regina Rensi2Simone Grassi3Barbara Gualco4Fabio Vaiano5Forensic Toxicology Laboratory, Department of Health Sciences, University of Florence, 50131 Firenze, ItalyForensic Toxicology Laboratory, Department of Health Sciences, University of Florence, 50131 Firenze, ItalyDivision of Forensic Legal Medicine, Department of Health Sciences, University of Florence, 50131 Firenze, ItalyDivision of Forensic Legal Medicine, Department of Health Sciences, University of Florence, 50131 Firenze, ItalyDivision of Forensic Legal Medicine, Department of Health Sciences, University of Florence, 50131 Firenze, ItalyForensic Toxicology Laboratory, Department of Health Sciences, University of Florence, 50131 Firenze, ItalyLysergic acid diethylamide (LSD) is a powerful hallucinogen. Its detection is limited by its low dosage; moreover, LSD is rapidly metabolized into 2-oxo-3-hydroxy-LSD (O-H-LSD). In this study we validated two methods for determination of LSD and O-H-LSD in blood. Method #1 consisted in the upgrade of a previously developed procedure for detection of 163 compounds. Method #2 was specific for LSD and O-H-LSD. Analyses were performed through LC-MS/MS by dynamic (#1) and/or MRM mode (#2), in positive ionization. Transitions were: 324→223,208 <i>m</i>/<i>z</i> for LSD; 356→237,222 <i>m</i>/<i>z</i> for O-H-LSD. Validations were performed following the AAFS’s guidelines. Linearity was good for both methods. Sensitivity was in line with previously validated methods with LOQs at 0.0375 (#1) and 0.025 (#2) ng/mL for LSD and 0.01875 (#1) and 0.0125 (#2) ng/mL for O-H-LSD. Bias and %CV always met the acceptance criteria. RRs were >83%, except for O-H-LSD with method #1. The methods were successfully applied to two real cases. Method #1 proved to be useful for screening purposes, while method #2 can represent a sensitive and reliable tool for confirmation procedures.https://www.mdpi.com/2297-8739/10/9/502LSDLC-MS/MSnew psychoactive substancesbloodscreening |
| spellingShingle | Alexandra Dimitrova Maria Grazia Di Milia Regina Rensi Simone Grassi Barbara Gualco Fabio Vaiano Determination of Lysergic Acid Diethylamide and 2-Oxo-3-Hydroxy-LSD in Blood: Validation and Comparison of Two Liquid Chromatography–Tandem Mass Spectrometry Methods Separations LSD LC-MS/MS new psychoactive substances blood screening |
| title | Determination of Lysergic Acid Diethylamide and 2-Oxo-3-Hydroxy-LSD in Blood: Validation and Comparison of Two Liquid Chromatography–Tandem Mass Spectrometry Methods |
| title_full | Determination of Lysergic Acid Diethylamide and 2-Oxo-3-Hydroxy-LSD in Blood: Validation and Comparison of Two Liquid Chromatography–Tandem Mass Spectrometry Methods |
| title_fullStr | Determination of Lysergic Acid Diethylamide and 2-Oxo-3-Hydroxy-LSD in Blood: Validation and Comparison of Two Liquid Chromatography–Tandem Mass Spectrometry Methods |
| title_full_unstemmed | Determination of Lysergic Acid Diethylamide and 2-Oxo-3-Hydroxy-LSD in Blood: Validation and Comparison of Two Liquid Chromatography–Tandem Mass Spectrometry Methods |
| title_short | Determination of Lysergic Acid Diethylamide and 2-Oxo-3-Hydroxy-LSD in Blood: Validation and Comparison of Two Liquid Chromatography–Tandem Mass Spectrometry Methods |
| title_sort | determination of lysergic acid diethylamide and 2 oxo 3 hydroxy lsd in blood validation and comparison of two liquid chromatography tandem mass spectrometry methods |
| topic | LSD LC-MS/MS new psychoactive substances blood screening |
| url | https://www.mdpi.com/2297-8739/10/9/502 |
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