Fast Residual Solvents and Terpenes Analyses in Cannabis and Hemp Products

New methodologies were developed for the analysis of residual solvents and terpenes using a single gas chromatography–mass spectrometry (GC–MS) system that are approximately 50% and 30% faster for the solvents and terpenes, respectively, compared to the original applications. This article describes the parameters for the implementation of the new methods on existing or new GC–MS systems. These methodologies offer laboratories the ability to run both residual solvent and terpenes analyses on a single platform without the need to change any consumable, such as liners and columns. The single platform-two analyses approach is ideal for start-up labs that may not be at full capacity while they ramp up sample volume. As a laboratory grows however, these methodologies are easily reimplemented on individual hardware platforms dedicated to a specific analysis. Both methods use helium as the carrier gas.

Residual solvents and terpenes analyses are integral applications for regulatory testing laboratories. These tests are to ensure compliance and provide a chemical fingerprint of the terpene profiles in myriad cannabis or hemp products. While residual solvent analysis is generally only applicable to more refined products derived from cannabis or hemp, terpenes analysis can be applied to almost any material ranging plant biomass to topical lotions and everything in between. The purpose of this work was to improve analytical efficiency and overall productivity on a single gas chromatography–mass spectrometry (GC–MS) platform using helium as carrier gas. The methodologies perform both residual solvent and terpenes analyses without the need to change any component of the GC–MS system. We have previously demonstrated the utility of this approach (1,2).

Materials and Methods

Please note, all part numbers provided in this section are specific to Agilent Technologies, Inc.Common hardware included:Intuvo 9000 Gas Chromatograph (G3950A) configured with a mid-column backflush FlowChip (option #881); multimode inlet (MMI) and guard chip (G4587-60665) or a split/splitless inlet (S/SL) and guard chip (G4587-60565); Agilent 7650A 50-position automatic liquid sampler (ALS) (G4567A); blue line ALS 10 µL syringe with PTFE tip (G4513-80220); a 4 mm ultra inert, low pressure drop, glass wool split liner (5190-2295); two DB-select 624 ultra inert columns (15 m X 0.25 mm I.D. x 1.4 µm film thickness [122-0314UI-INT]); and a 7697A headspace sampler configured with a 0.5 mL loop (G45556-80105) and two loop adaptors (G4556-20177). XLSI weldment was used for side mount of the 7697A headspace sampler transfer line (G3969A). In addition, a 5-m deactivated DB-ProSteel transfer line (160-4535-5) was used. An Agilent 5977B mass selective detector (MSD) with extractor EI source (G7077BA or G7076BA) with a 9 mm extractor lens (G3870-20449) was also used. Agilent Mass Hunter software was used for data acquisition and quantitative analysis. See Tables I–X for method conditions.

Results and Discussion

This work built upon and improved prior art for the analysis of residual solvents and terpenes in cannabis and hemp matrices. The primary intent was to improve efficiency and productivity using helium as a carrier gas for a single platform to perform both analyses without the need to change any hardware or consumables. The terpenes method used liquid injection and the solvents method employed headspace—all through a single GC inlet on the GC–MS system. The resulting methodologies met or exceeded the limits of detection, limits of quantitation, accuracy, and precision as the original referenced methods. Chromatographic examples are provided in the Figures 1–5.

Conclusion

This work developed and verified method parameters for the analysis of residual solvents and terpenes in cannabinoid and hemp products using the Agilent 7697A-Intuvo 9000/5977B headspace-GC–MS system with liquid injection. The hardware and consumables offer a single platform that can analyze both chemotypes. Accuracy, precision, range, linearity, limits of detection, and quantitation met or exceeded those of the previous work developed in our laboratories. This new, and novel analytical approach has already been successfully implemented in laboratories across North America.

Disclaimer

Agilent products and solutions are intended to be used for cannabis quality control and safety testing in laboratories where such use is permitted under state and country law (DE17556094).

References

1. Hollis, J.S., Harper, T., and Macherone, A., Terpenes Analysis in Cannabis Products by Liquid Injection using the Agilent Intuvo 9000/5977B GC/MS System. Agilent application note 5994-2032EN. Agilent Technologies, Inc., 2020.
2. Harper, T., Hollis, J.S., and Macherone, A., Novel Residual Solvents Analysis of Cannabinoid Products with the Agilent Headspace-GC/MS System. Agilent application note 5994-1926EN. Agilent Technologies, Inc., 2020.

About the Authors

Anthony Macherone, PhD, was the Strategic Technical Scientist with Agilent Technologies. His expertise in the application of LC–MS and GC–MS methodologies in drug discovery and medicinal chemistry, metabolomics, and exposomics. For the past 6+ years, Anthony led a team of Agilent scientists for the development, deployment, and support of analytical testing methodologies for cannabis and hemp products. Jeffery S. Hollis is a Senior Applications Chemist for GC–MS systems with Agilent Technologies.

How to Cite This Article

Hollis, J., Macherone, A., Fast Residual Solvents and Terpenes Analyses in Cannabis and Hemp Products, Cannabis Science and Technology, 2024, 7(1), 26-28.