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      Analysis of 2,5-dimethoxy-amphetamines and 2,5-dimethoxy-phenethylamines aiming their determination in biological matrices: a review

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          Abstract

          Purpose

          The present review aims to provide an overview of methods for the quantification of 2,5-dimethoxy-amphetamines and -phenethylamines in different biological matrices, both traditional and alternative ones.

          Methods

          A complete literature search was carried out with PubMed, Scopus and the World Wide Web using relevant keywords, e.g., designer drugs, amphetamines, phenethylamines, and biological matrices.

          Results

          Synthetic phenethylamines represent one of the largest classes of “designer drugs”, obtained through chemical structure modifications of psychoactive substances to increase their pharmacological activities. This practice is also favored by the fact that every new synthetic compound is not considered illegal by existing legislation. Generally, in a toxicological laboratory, the first monitoring of drugs of abuse is made by rapid screening tests that sometimes can occur in false positive or false negative results. To reduce evaluation errors, it is mandatory to submit the positive samples to confirmatory methods, such as gas chromatography or liquid chromatography combined to mass spectrometry, for a more specific qualitative and quantitative analysis.

          Conclusions

          This review highlights the great need for updated comprehensive analytical methods, particularly when analyzing biological matrices, both traditional and alternative ones, for the search of newly emerging designer drugs.

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          Most cited references139

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          Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS.

          B Matuszewski, M L Constanzer, C. M. Chavez-Eng (2003)
          In recent years, high-performance liquid chromatography (HPLC) with tandem mass spectrometric (MS/MS) detection has been demonstrated to be a powerful technique for the quantitative determination of drugs and metabolites in biological fluids. However, the common and early perception that utilization of HPLC-MS/MS practically guarantees selectivity is being challenged by a number of reported examples of lack of selectivity due to ion suppression or enhancement caused by the sample matrix and interferences from metabolites. In light of these serious method liabilities, questions about how to develop and validate reliable HPLC-MS/MS methods, especially for supporting long-term human pharmacokinetic studies, are being raised. The central issue is what experiments, in addition to the validation data usually provided for the conventional bioanalytical methods, need to be conducted to confirm HPLC-MS/MS assay selectivity and reliability. The current regulatory requirements include the need for the assessment and elimination of the matrix effect in the bioanalytical methods, but the experimental procedures necessary to assess the matrix effect are not detailed. Practical, experimental approaches for studying, identifying, and eliminating the effect of matrix on the results of quantitative analyses by HPLC-MS/MS are described in this paper. Using as an example a set of validation experiments performed for one of our investigational new drug candidates, the concepts of the quantitative assessment of the "absolute" versus "relative" matrix effect are introduced. In addition, experiments for the determination of, the "true" recovery of analytes using HPLC-MS/MS are described eliminating the uncertainty about the effect of matrix on the determination of this commonly measured method parameter. Determination of the matrix effect allows the assessment of the reliability and selectivity of an existing HPLC-MS/MS method. If the results of these studies are not satisfactory, the parameters determined may provide a guide to what changes in the method need to be made to improve assay selectivity. In addition, a direct comparison of the extent of the matrix effect using two different interfaces (a heated nebulizer, HN, and ion spray, ISP) under otherwise the same sample preparation and chromatographic conditions was made. It was demonstrated that, for the investigational drug under study, the matrix effect was clearly observed when ISP interface was utilized but it was absent when the HN interface was employed.
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            Validation of new methods.

            Olaf H Drummer, Brian Peters, Frank Musshoff (2007)
            Reliable analytical data are a prerequisite for correct interpretation of toxicological findings in the evaluation of scientific studies, as well as in daily routine work. Unreliable analytical data might not only be contested in court, but could also lead to unjustified legal consequences for the defendant or to wrong treatment of the patient. Therefore, new analytical methods to be used in forensic and/or clinical toxicology require careful method development and thorough validation of the final method. This is especially true in the context of quality management and accreditation, which have become matters of increasing relevance in analytical toxicology in recent years. In this paper, important considerations in analytical method validation will be discussed which may be used as guidance by scientists wishing to develop and validate analytical methods.
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              Trends in quality in the analytical laboratory. II. Analytical method validation and quality assurance

              Isabel Taverniers, Marc De Loose, Erik Van Bockstaele (2004)
              Article 0 comments Cited 107 times – based on 0 reviews     Review now
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                Author and article information

                Contributors
                Maria Nieddu:
                ORCID: http://orcid.org/0000-0001-7589-0464
                marvi@uniss.it
                Journal
                Journal ID (nlm-ta): Forensic Toxicol
                Journal ID (iso-abbrev): Forensic Toxicol
                Title: Forensic Toxicology
                Publisher: Springer Nature Singapore (Singapore )
                ISSN (Print): 1860-8965
                ISSN (Electronic): 1860-8973
                Publication date (Electronic): 14 September 2022
                Publication date PMC-release: 14 September 2022
                Publication date (Print): 2023
                Volume: 41
                Issue: 1
                Pages: 1-24
                Affiliations
                [1 ]GRID grid.11450.31, ISNI 0000 0001 2097 9138, Department of Chemistry and Pharmacy, , University of Sassari, ; 07100 Sassari, Italy
                [2 ]GRID grid.11450.31, ISNI 0000 0001 2097 9138, Department of Veterinary Medicine, , University of Sassari, ; 07100 Sassari, Italy
                [3 ]GRID grid.4691.a, ISNI 0000 0001 0790 385X, Department of Pharmacy, , University of Naples Federico II, ; 80131 Naples, Italy
                Author information
                http://orcid.org/0000-0001-7589-0464
                Article
                Publisher ID: 638
                DOI: 10.1007/s11419-022-00638-6
                PMC ID: 9849320
                PubMed ID: 36652064
                SO-VID: 2803cb8f-6a4f-4cdb-b587-304f7a9eb5af
                Copyright © © The Author(s) 2022
                License:

                Open AccessThis article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons licence, and indicate if changes were made. The images or other third party material in this article are included in the article's Creative Commons licence, unless indicated otherwise in a credit line to the material. If material is not included in the article's Creative Commons licence and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this licence, visit http://creativecommons.org/licenses/by/4.0/.

                History
                Date received : 19 May 2022
                Date accepted : 19 August 2022
                Funding
                Funded by: “Fondo di Ateneo per la ricerca 2019” of Sassari University
                Funded by: Università degli Studi di Sassari
                Open Access :

                Open access funding provided by Università degli Studi di Sassari within the CRUI-CARE Agreement.

                Categories
                Subject: Review Article
                Custom metadata
                issue-copyright-statement © The Author(s), under exclusive licence to Japanese Association of Forensic Toxicology 2023

                Keywords: 2,5-dimethoxy-amphetamines and -phenethylamines,hallucinatory designer drugs,biological matrices,lc–ms/ms,gc–ms/ms
                Data availability:
                Keywords: 2,5-dimethoxy-amphetamines and -phenethylamines, hallucinatory designer drugs, biological matrices, lc–ms/ms, gc–ms/ms

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