[Structure Analysis and Characterization of Aminorex Analogue 4'-F-4-MAR].
Fa Yi Xue Za Zhi
; 36(5): 677-681, 2020 Oct.
Article
em Zh
| MEDLINE
| ID: mdl-33295170
ABSTRACT
ABSTRACT Objective To study the identification method for 4'-F-4-methylaminorex ï¼4'-F-4-MARï¼ in samples without reference substance. Methods Gas chromatography-mass spectrometry ï¼GC-MSï¼, ultra-high-performance liquid chromatography-quadrupole time-of-flight-mass spectrometry ï¼UPLC-QTOF-MSï¼, nuclear magnetic resonance ï¼NMRï¼ and Fourier transform infrared ï¼FTIRï¼ were comprehensively used for the structure identification of 4'-F-4-MAR in samples. Results Under the positive electrospray ionization ï¼ESI+ï¼ mode, quasi-molecular ion in the first order mass spectrometry of the unknown compound was 195.092 6 and its molecular formula was inferred to be C10H11FN2O. The fragment ions in the mass spectrometry of the unknown compound were compared with the related fragment ions of 4,4'-dimethylaminorex ï¼4,4'-DMARï¼ in literature. It was found that the main fragment ions of the unknown compound were all 4 bigger than the corresponding fragment ions of 4,4'-DMAR. Therefore, the unknown compound was inferred to be a 4,4'-DMAR analogue with a methyl substituted by a fluorine in the benzene ring. The equivalent protons at δ=7.30 and δ=7.06 in 1H-nuclear magnetic resonance ï¼1H-NMRï¼ spectra and the characteristic spin-spin coupling constants ï¼1JC-F=245.2 Hz, 2JC-F=21.3 Hz, 3JC-F=8.1 Hzï¼ for 13C-19F interactions in carbon spectra, further proved that the fluorine substituted methyl at the para-position of the benzene ring. Finally, the unknown compound was determined as 4'-F-4-MAR. Conclusion A method that comprehensively used the identification materials 4'-F-4-MAR in GC-MS, UPLC-QTOF-MS, NMR and FTIR is established and the fragmentation mechanism of fragmentation ions of 4'-F-4-MAR created under the two modes -- electron impact ï¼EIï¼ and electrospray ionization under collision induced dissociation ï¼ESI-CIDï¼ is deduced. The information will assist forensic science laboratories in identifying this compound or other substances with similar structure in their case work.
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Texto completo:
1
Coleções:
01-internacional
Base de dados:
MEDLINE
Assunto principal:
Espectrometria de Massas por Ionização por Electrospray
/
Aminorex
Tipo de estudo:
Prognostic_studies
Idioma:
Zh
Revista:
Fa Yi Xue Za Zhi
Assunto da revista:
JURISPRUDENCIA
Ano de publicação:
2020
Tipo de documento:
Article
País de afiliação:
China