Rapid identification of novel psychoactive and other controlled substances using low-field 1H NMR spectroscopy

Lysbeth H. Antonides; Rachel M. Brignall; Andrew Costello; Jamie Ellison; Samuel E. Firth; Nicolas Gilbert; Bethany J. Groom; Samuel J. Hudson; Matthew C. Hulme; Jack Marron; Zoe A. Pullen; Thomas B. R. Robertson; Christopher J. Schofield; David C. Williamson; E. Kate Kemsley; Oliver B. Sutcliffe; Ryan E. Mewis

doi:10.1021/acsomega.9b00302

Rapid identification of novel psychoactive and other controlled substances using low-field ¹H NMR spectroscopy

Lysbeth H. Antonides, Rachel M. Brignall, Andrew Costello, Jamie Ellison, Samuel E. Firth, Nicolas Gilbert, Bethany J. Groom, Samuel J. Hudson, Matthew C. Hulme, Jack Marron, Zoe A. Pullen, Thomas B. R. Robertson, Christopher J. Schofield, David C. Williamson, E. Kate Kemsley, Oliver B. Sutcliffe, Ryan E. Mewis

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Abstract

An automated approach to the collection of H-1 NMR (nuclear magnetic resonance) spectra using a benchtop NAIR spectrometer and the subsequent analysis, processing, and elucidation of components present in seized drug samples are reported. An algorithm is developed to compare spectral data to a reference library of over 300 H-1 NMR spectra, ranking matches by a correlation-based score. A threshold for identification was set at 0.838, below which identification of the component present was deemed unreliable. Using this system, 432 samples were surveyed and validated against contemporaneously acquired GC-MS (gas chromatography-mass spectrometry) data. Following removal of samples which possessed no peaks in the GC-MS trace or in both the NMR spectrum and GC-MS trace, the remaining 416 samples matched in 93% of cases. Thirteen of these samples were binary mixtures. A partial match (one component not identified) was obtained for 6% of samples surveyed whilst only 1% of samples did not match at all.

Original language	English
Pages (from-to)	7103-7112
Number of pages	10
Journal	ACS Omega
Volume	4
Issue number	4
Early online date	19 Apr 2019
DOIs	https://doi.org/10.1021/acsomega.9b00302
Publication status	Published - 30 Apr 2019

Keywords

RAMAN-SPECTROSCOPY
SYNTHETIC CANNABINOIDS
LIQUID-CHROMATOGRAPHY
HERBAL MIXTURES
LEGAL HIGHS
GC-MS
DRUGS
QUANTIFICATION
FIELD
DIFFERENTIATION

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10.1021/acsomega.9b00302Licence: CC BY-NC-ND

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Cite this

Antonides, L. H., Brignall, R. M., Costello, A., Ellison, J., Firth, S. E., Gilbert, N., Groom, B. J., Hudson, S. J., Hulme, M. C., Marron, J., Pullen, Z. A., Robertson, T. B. R., Schofield, C. J., Williamson, D. C., Kemsley, E. K., Sutcliffe, O. B., & Mewis, R. E. (2019). Rapid identification of novel psychoactive and other controlled substances using low-field ¹H NMR spectroscopy. ACS Omega, 4(4), 7103-7112. https://doi.org/10.1021/acsomega.9b00302

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title = "Rapid identification of novel psychoactive and other controlled substances using low-field 1H NMR spectroscopy",

abstract = "An automated approach to the collection of H-1 NMR (nuclear magnetic resonance) spectra using a benchtop NAIR spectrometer and the subsequent analysis, processing, and elucidation of components present in seized drug samples are reported. An algorithm is developed to compare spectral data to a reference library of over 300 H-1 NMR spectra, ranking matches by a correlation-based score. A threshold for identification was set at 0.838, below which identification of the component present was deemed unreliable. Using this system, 432 samples were surveyed and validated against contemporaneously acquired GC-MS (gas chromatography-mass spectrometry) data. Following removal of samples which possessed no peaks in the GC-MS trace or in both the NMR spectrum and GC-MS trace, the remaining 416 samples matched in 93% of cases. Thirteen of these samples were binary mixtures. A partial match (one component not identified) was obtained for 6% of samples surveyed whilst only 1% of samples did not match at all.",

keywords = "RAMAN-SPECTROSCOPY, SYNTHETIC CANNABINOIDS, LIQUID-CHROMATOGRAPHY, HERBAL MIXTURES, LEGAL HIGHS, GC-MS, DRUGS, QUANTIFICATION, FIELD, DIFFERENTIATION",

author = "Antonides, {Lysbeth H.} and Brignall, {Rachel M.} and Andrew Costello and Jamie Ellison and Firth, {Samuel E.} and Nicolas Gilbert and Groom, {Bethany J.} and Hudson, {Samuel J.} and Hulme, {Matthew C.} and Jack Marron and Pullen, {Zoe A.} and Robertson, {Thomas B. R.} and Schofield, {Christopher J.} and Williamson, {David C.} and Kemsley, {E. Kate} and Sutcliffe, {Oliver B.} and Mewis, {Ryan E.}",

year = "2019",

month = apr,

day = "30",

doi = "10.1021/acsomega.9b00302",

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Antonides, LH, Brignall, RM, Costello, A, Ellison, J, Firth, SE, Gilbert, N, Groom, BJ, Hudson, SJ, Hulme, MC, Marron, J, Pullen, ZA, Robertson, TBR, Schofield, CJ, Williamson, DC, Kemsley, EK, Sutcliffe, OB & Mewis, RE 2019, 'Rapid identification of novel psychoactive and other controlled substances using low-field ¹H NMR spectroscopy', ACS Omega, vol. 4, no. 4, pp. 7103-7112. https://doi.org/10.1021/acsomega.9b00302

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T1 - Rapid identification of novel psychoactive and other controlled substances using low-field 1H NMR spectroscopy

AU - Antonides, Lysbeth H.

AU - Brignall, Rachel M.

AU - Costello, Andrew

AU - Ellison, Jamie

AU - Firth, Samuel E.

AU - Gilbert, Nicolas

AU - Groom, Bethany J.

AU - Hudson, Samuel J.

AU - Hulme, Matthew C.

AU - Marron, Jack

AU - Pullen, Zoe A.

AU - Robertson, Thomas B. R.

AU - Schofield, Christopher J.

AU - Williamson, David C.

AU - Kemsley, E. Kate

AU - Sutcliffe, Oliver B.

AU - Mewis, Ryan E.

PY - 2019/4/30

Y1 - 2019/4/30

N2 - An automated approach to the collection of H-1 NMR (nuclear magnetic resonance) spectra using a benchtop NAIR spectrometer and the subsequent analysis, processing, and elucidation of components present in seized drug samples are reported. An algorithm is developed to compare spectral data to a reference library of over 300 H-1 NMR spectra, ranking matches by a correlation-based score. A threshold for identification was set at 0.838, below which identification of the component present was deemed unreliable. Using this system, 432 samples were surveyed and validated against contemporaneously acquired GC-MS (gas chromatography-mass spectrometry) data. Following removal of samples which possessed no peaks in the GC-MS trace or in both the NMR spectrum and GC-MS trace, the remaining 416 samples matched in 93% of cases. Thirteen of these samples were binary mixtures. A partial match (one component not identified) was obtained for 6% of samples surveyed whilst only 1% of samples did not match at all.

AB - An automated approach to the collection of H-1 NMR (nuclear magnetic resonance) spectra using a benchtop NAIR spectrometer and the subsequent analysis, processing, and elucidation of components present in seized drug samples are reported. An algorithm is developed to compare spectral data to a reference library of over 300 H-1 NMR spectra, ranking matches by a correlation-based score. A threshold for identification was set at 0.838, below which identification of the component present was deemed unreliable. Using this system, 432 samples were surveyed and validated against contemporaneously acquired GC-MS (gas chromatography-mass spectrometry) data. Following removal of samples which possessed no peaks in the GC-MS trace or in both the NMR spectrum and GC-MS trace, the remaining 416 samples matched in 93% of cases. Thirteen of these samples were binary mixtures. A partial match (one component not identified) was obtained for 6% of samples surveyed whilst only 1% of samples did not match at all.

KW - RAMAN-SPECTROSCOPY

KW - SYNTHETIC CANNABINOIDS

KW - LIQUID-CHROMATOGRAPHY

KW - HERBAL MIXTURES

KW - LEGAL HIGHS

KW - GC-MS

KW - DRUGS

KW - QUANTIFICATION

KW - FIELD

KW - DIFFERENTIATION

U2 - 10.1021/acsomega.9b00302

DO - 10.1021/acsomega.9b00302

M3 - Article

SN - 2470-1343

VL - 4

SP - 7103

EP - 7112

JO - ACS Omega

JF - ACS Omega

IS - 4

ER -