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![]() Life Sci 97:78–90Īuwärter V, Dresen S, Weinmann W, Müller M, Pütz M, Ferreirós N (2009) ‘Spice’ and other herbal blends: harmless incense or cannabinoid designer drugs? J Mass Spectrom 44:832–837 Anal Chim Acta 874:11–25ĮlSohly MA, Gul W, Wanas AS, Radwan MM (2014) Synthetic cannabinoids: analysis and metabolites. Znaleziona J, Ginterová P, Petr J, Ondra P, Válka I, Sevčic J, Chrastina J, Maier V (2015) Determination and identification of synthetic cannabinoids and their metabolites in different matrices by modern analytical techniques-a review. doi: 10.2810/372415īrewer TI, Collins M (2014) A review of clinical manifestations in adolescent and young adults after use of synthetic cannabinoids. doi: 10.2810/27063Įuropean Monitoring Centre for Drugs and Drug Addiction (EMCDDA) (2015) New psychoactive substances in Europe: an update from the EU Early Warning System, Luxembourg. Forensic Sci Int 191:58–63Įuropean Monitoring Centre for Drugs and Drug Addiction (EMCDDA) (2009) Understanding the 'Spice' phenomenon, Luxembourg. Lindigkeit R, Boehme A, Eiserloh I, Luebbecke M, Wiggermann M, Ernst L, Beuerle T (2009) Spice: a never ending story. Herewith, we report analytical characteristics of CUMYL-4CN-BINACA enabling its (and possible analogues thereof) determination in criminal seizures. On the basis of the spectral data, the compound was identified as CUMYL-4CN-BINACA. All protons and carbons were assigned by their couplings and correlations observed in 1H- 1H correlation spectroscopy, 1H- 13C heteronuclear multiple bond correlation, and 1H- 13C heteronuclear single quantum coherence spectra. The GC–MS, FT-IR and 1H and 13C NMR spectra of the compound coincided well with the reference data. Pure compound was analyzed by gas chromatography–mass spectrometry (GC–MS), attenuated total reflection Fourier-transform infrared spectroscopy (FT-IR), and one- and two-dimensional nuclear magnetic resonance (NMR) spectroscopy. The extract was purified by column chromatography. To elucidate the chemical structure, the dried herbal mixture was extracted with methanol. If high 13C resolution is not critical then run an HMQC.We were the first to detect N-(2-phenylpropan-2-yl)-1-(4-cyanobutyl)-1 H-indazole-3-carboxamide (common name CUMYL-4CN-BINACA) as a new synthetic cannabinoid, on the illegal market in Bursa, Turkey. My advice to students is that, if high 13C resolution is required, then make sure the pulses are calibrated well on a well tuned and matched probe and run an HSQC. This is definitely the case if all of the pulses are calibrated well, however since there are many more pulses in an HSQC compared to an HMQC, it is more susceptible to losses in signal-to-noise-ratio due to poor probe tuning or poor pulse calibration. One might conclude that, due to the higher 13C resolution, it is always better to run an HSQC rather than an HMQC. One can see that the resolution is better in the projection of the HSQC compared to the HMQC. The bottom panel of the figure shows the corresponding 13C projection spectra. One can see that the expanded cross peak of the HMQC is broader in the 13C dimension than that of the HSQC. The top panel of the figure below shows the 7.05 T 1H / 13C HMQC and HSQC spectra of menthol with an expansion of one of the resonances highlighted in yellow. The homonuclear proton J coupling manifests itself as broadening in the X dimension. This means that an HMQC is affected by homonuclear proton J coupling during the evolution period while an HSQC is not affected as there is no proton magnetization during the evolution time. The difference between the two techniques is that during the evolution time of an HMQC both proton and X magnetization (eg: X = 13C ) are allowed to evolve whereas in an HSQC only X magnetization is allowed to evolve. Since both techniques essentially provide the same information - a correlation map between the coupled spins - students sometimes ask which of these two methods is better and which should they use routinely. Proton detected Heteronuclear Multiple Quantum Coherence (HMQC) and Heteronuclear Single Quantum Coherence (HSQC) are both NMR techniques used to correlate the chemical shift of the protons in a sample to a heteronucleus such as 13C or 15N via the J coupling interaction between the nuclei. ![]()
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