ICRS: CHARACTERISATION OF DELTA-8 THC DISTILLATES USING HIGH RESOLUTION MASS SPECTROMETRY (HRMS) AND CYCLIC ION MOBILITY SPECTROMETRY COUPLED WITH HRMS

Significance of the topic

Delta-8-THC is an increasingly common cannabinoid in consumer products, raising safety and regulatory concerns. Analytical methods to characterize Δ8-THC distillates and byproducts are essential for product quality and compliance.

Objectives and study overview

This work demonstrates the application of high-resolution mass spectrometry (HRMS) and cyclic ion mobility spectrometry (cIMS) to identify and resolve isomeric and halogenated byproducts in Δ8-THC distillates derived from CBD.

Methodology

• Sample preparation: Distillate samples dissolved in acetonitrile; positive-mode electrospray ionization.
• Chromatography: UPLC with CORTECS C18 column (2.1×100 mm, 1.6 μm), mobile phases 0.1% formic acid in water and acetonitrile, 0.56 mL/min flow rate, 25 °C.
• Mass spectrometry: Xevo G3 QTOF in MSE mode for simultaneous low and high collision energy scans.
• Ion mobility: Single-pass and multi-pass separations using a travelling-wave cyclic IMS device.

Used instrumentation

• Waters ACQUITY UPLC I-Class Plus
• Waters Xevo G3 QTOF
• Waters Select Series Cyclic IMS
• Software: UNIFI and MassLynx

Key results and discussion

• HRMS analysis detected major cannabinoids and multiple unknown components with base peak m/z 315.2318 attributed to C21H30O2 isomers eluting before Δ8-THC.
• Single-pass IMS did not separate CBL and (6aR,9S)-Δ10-THC, but multi-pass IMS (six passes) achieved baseline resolution of co-eluting isomers, revealing additional peaks.
• A chlorinated byproduct (m/z 351.2080) was identified as C21H31ClO2 with ~19% area, indicating <80% sample purity.
• Post-IMS collision-induced dissociation provided clean MS/MS spectra for mobility-separated precursors, aiding structural elucidation.

Benefits and practical applications

• Improved isomer resolution enhances quality control and regulatory compliance in cannabinoid products.
• cIMS–MS workflows enable rapid differentiation of co-eluting impurities without extended chromatographic methods.
• Detection of halogenated species emphasizes the need to monitor synthetic byproducts for safety.

Future trends and potential applications

• Integration of IMS with other separation techniques for comprehensive botanical extract profiling.
• Development of standardized IMS libraries for rapid cannabinoid identification.
• Automation of multi-pass IMS workflows to improve throughput in high-volume testing environments.

Conclusion

The combination of high-resolution QTOF MS and cyclic IMS effectively characterizes Δ8-THC distillates, resolving isomeric and halogenated byproducts. Multi-pass IMS enhances separation power, while post-IMS MS/MS offers detailed structural insights, providing a robust platform for cannabinoid quality assurance.

Reference

1. Erickson BE. Delta-8-THC craze concerns chemists. Chem Eng News. 2021;99(31).
2. Hudalla C. We believe in unicorns (and Delta-8). The Cannabis Scientist. 2021.
3. Golombek P, et al. Conversion of CBD into psychotropic cannabinoids. Toxics. 2020;8(2).
4. Kiselak TD, et al. Synthetic route sourcing of illicit CBD isomerization. Forensic Sci Int. 2020;308:110173.
5. Watanabe K, et al. Conversion of CBD to Δ9-THC in artificial gastric juice. Forensic Toxicol. 2007;25(1):16-21.
6. Meehan-Atrash J, Rahman I. Novel Δ8-THC vaporizers contain unlabeled adulterants. Chem Res Toxicol. 2022;35(1):73-76.
7. Webster GRB, Sarna LP, Mechoulam R. US Patent US20040143126A1.
8. Giles K, et al. A cyclic ion mobility–mass spectrometry system. Anal Chem. 2019;91(13):8564-8573.