Quantitative NMR as a tool for analysis of new psychoactive substances

Serrano, Julia Neves Prates; Benedito, Luiz Eduardo Celino; Souza, Mônica P.; Maldaner, Adriano O.; Oliveira, Aline

doi:10.1016/j.forc.2020.100282

Cited by 14 publications

(16 citation statements)

References 19 publications

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“…NMR is a powerful analytical technique that enables acquisition of data relating more specifically to the molecular structure and tridimensional disposition of atoms (Bono, 2007). High‐field NMR is a powerful technique that has been underutilized in drug analysis (Hussain et al, 2020; Serrano et al, 2020) but it seem to be drawing more interest of the forensic community in the analysis of NPS, especially when no reference material is available for comparison. This technique provides unequivocal structure determination (Castaing‐Cordier et al, 2021; Serrano et al, 2020) and it can be performed using different modes such as one‐dimensional proton ( 1 H) and carbon ( 13 C) NMR and two‐dimensional correlation NMR (e.g., homonuclear correlation spectroscopy [COSY], nuclear overhauser effect spectroscopy [NOESY], and HMQC) (Bono, 2007; UNODC, 2020b).…”

Section: Nuclear Magnetic Ressonancementioning

confidence: 99%

“…High‐field NMR is a powerful technique that has been underutilized in drug analysis (Hussain et al, 2020; Serrano et al, 2020) but it seem to be drawing more interest of the forensic community in the analysis of NPS, especially when no reference material is available for comparison. This technique provides unequivocal structure determination (Castaing‐Cordier et al, 2021; Serrano et al, 2020) and it can be performed using different modes such as one‐dimensional proton ( 1 H) and carbon ( 13 C) NMR and two‐dimensional correlation NMR (e.g., homonuclear correlation spectroscopy [COSY], nuclear overhauser effect spectroscopy [NOESY], and HMQC) (Bono, 2007; UNODC, 2020b). Fast analyses, high reproducibility, and minimal low sample preparation are some of the analytical advantages offered by NMR (Santos et al, 2018; Serrano et al, 2020), without requiring any prior separation (Ribeiro et al, 2018).…”

Section: Nuclear Magnetic Ressonancementioning

confidence: 99%

“…This technique provides unequivocal structure determination (Castaing‐Cordier et al, 2021; Serrano et al, 2020) and it can be performed using different modes such as one‐dimensional proton ( 1 H) and carbon ( 13 C) NMR and two‐dimensional correlation NMR (e.g., homonuclear correlation spectroscopy [COSY], nuclear overhauser effect spectroscopy [NOESY], and HMQC) (Bono, 2007; UNODC, 2020b). Fast analyses, high reproducibility, and minimal low sample preparation are some of the analytical advantages offered by NMR (Santos et al, 2018; Serrano et al, 2020), without requiring any prior separation (Ribeiro et al, 2018). Analysis by NMR is nondestructive (Castaing‐Cordier et al, 2021; Ribeiro et al, 2018; Santos et al, 2018) and can enable the determination of multiple compounds within the same analysis (Castaing‐Cordier et al, 2021).…”

Section: Nuclear Magnetic Ressonancementioning

confidence: 99%

“…Analysis by NMR is nondestructive (Castaing‐Cordier et al, 2021; Ribeiro et al, 2018; Santos et al, 2018) and can enable the determination of multiple compounds within the same analysis (Castaing‐Cordier et al, 2021). In addition, NMR analyses of synthetic cathinones can provide important structural data when certified reference materials are unavailable (Guirguis et al, 2017; Serrano et al, 2020). One of the great potentialities of NMR is that the identification of a single drug or a mixture as well as the differentiation of constitutional isomers can be performed (Bono, 2007; Castaing‐Cordier et al, 2021; UNODC, 2020b).…”

Section: Nuclear Magnetic Ressonancementioning

confidence: 99%

See 3 more Smart Citations

Identification of synthetic cathinones in seized materials: A review of analytical strategies applied in forensic chemistry

Campos

Krotulski

Martinis

et al. 2022

WIREs Forensic Science

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Synthetic cathinones are a class of novel psychoactive substances, commonly tested in seized materials by forensic chemistry laboratories. These drugs have been found in different types of seized materials including powders, tablets, liquids, herbs, and blotters. A comprehensive review of the literature shows that the analyses of synthetic cathinones have been performed by a diverse repertoire of techniques, from more traditional to emerging methods. Techniques commonly used in the analysis of "traditional" illicit drugs, such as color and microcrystalline tests, chromatography, capillary electrophoresis, mass spectrometry (MS), and infrared (IR), and Raman spectroscopies, have been used for screening and/or confirmatory purposes, depending on the technique and laboratories preference. However, other emerging techniques, such as nuclear magnetic resonance, high-resolution MS, direct analysis in real-time MS, gas chromatography with IR detection, and so on, have been drawing the attention of forensic scientists due to the advantages of these techniques in providing important structural data. It is important to consider that each technique presents analytical benefits and limitations, which should be considered when analyzing synthetic cathinones in seized materials. Furthermore, the combination of more than one analytical technique is always recommended, especially when an unknown synthetic cathinone is suspected and/or encountered in the sample.

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Section: Nuclear Magnetic Ressonancementioning

confidence: 99%

Section: Nuclear Magnetic Ressonancementioning

confidence: 99%

Section: Nuclear Magnetic Ressonancementioning

confidence: 99%

Section: Nuclear Magnetic Ressonancementioning

confidence: 99%

See 2 more Smart Citations

Identification of synthetic cathinones in seized materials: A review of analytical strategies applied in forensic chemistry

Campos

Krotulski

Martinis

et al. 2022

WIREs Forensic Science

View full text Add to dashboard Cite

show abstract

“…The reported commonly used quantitative method for synthetic cannabinoid in herbal blends were HPLC [13], ultra-HPLC (UHPLC) [14], GC-MS [7], and NMR [15][16][17][18]. The NMR has many advantages especially in the absence of certified reference materials.…”

Section: Introductionmentioning

confidence: 99%

Identification and quantification of 10 indole/indazole carboxamide synthetic cannabinoids in 36 herbal blends by gas chromatography‐mass spectrometry and nuclear magnetic resonance spectroscopy

Liu

Wang

Meng

et al. 2021

Journal of Forensic Sciences

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Herbal blends containing synthetic cannabinoids have become popular alternatives to marijuana. The number of synthetic cannabinoids and speed of their emergence enable this group of compounds particularly challenging in terms of detection, monitoring, and responding. In this work, both gas chromatography-mass spectrometry (GC-MS) and nuclear magnetic resonance spectroscopy (NMR) methods were developed for the identification and quantification of synthetic cannabinoids in herbal blends. Ten types of indole/indazole carboxamide synthetic cannabinoids, which showed different types of substitutions connected to nitrogen of the indole/indazole carboxamide, were detected in 36 herbal blends. The GC-MS fragmentation routes of indole/indazole carboxamide synthetic cannabinoids were discussed in detail for structure identification purpose. The concentration range of synthetic cannabinoid in 36 herbal blends was 1.9-50.6 mg/g using GC-MS method, while 1.5-49.0 mg/g by NMR method. Nicotine in herbal blends was quantified by NMR method without using reference material, and showed a variation of 5.3-44.7 mg/g. For quantitative analysis, NMR method showed great advantage in the absence of reference material, while GC-MS method showed great merit for multiple-compound analysis when reference material was available. Therefore, for the quantitative analysis of new emerged synthetic cannabinoid in herbal blends, different methods could be chosen by considering whether reference material is available, as well as the number and types of synthetic cannabinoids detected in a single sample.

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