SPME-GC/MS of Selected Terpenes Using Agilent DVB/CAR-WR/PDMS SPME Fiber

Significance of the topic

The widespread legalization of cannabis has intensified the need for accurate, rapid, and cost-effective profiling of terpenes to ensure product quality, safety, and consistency in commercial and research laboratories.

• Eliminates the use of organic solvents
• Reduces coextraction of matrix interferences
• Enables peak confirmation through mass spectral data

Study objectives and overview

This proof-of-principle study demonstrates the capabilities of static headspace SPME-GC/MS using an 80/10 µm DVB/CAR/PDMS fiber for qualitative and semi-quantitative analysis of selected terpenes in cannabis flower. The main goals include assessing fiber reproducibility, achieving rapid volatile extraction, and generating reliable spectral identification.

Methodology

Solid phase microextraction was conducted on 20 mL headspace vials containing either a 5 ppm terpene standard solution or 0.1 g of homogenized cannabis flower with 8 mL of Milli-Q water. Samples were incubated at 40 °C for 5 minutes with stirring at 1 000 rpm, followed by a 20 minute extraction using an 80/10 µm DVB/CAR/PDMS fiber. Thermal desorption to the GC inlet was performed at 270 °C for 3 minutes prior to chromatographic analysis.

Used instrumentation

• Agilent PAL RTC autosampler in SPME Arrow configuration
• DVB/CAR/PDMS SPME fiber (p/n 5191-5874)
• Agilent 7890B GC with splitless Ultra Inert liner and 60 m DB-1ms column (0.25 mm ID, 0.25 µm film)
• Agilent 5977B MSD with high efficiency source
• Heatex Stirrer 1 set to 40 °C and 1 000 rpm agitation

Main results and discussion

Reproducibility tests involving 12 replicate injections on three fibers yielded percent RSDs below 20% for all target terpenes, with averages ranging from 3.3% for limonene to 19.1% for guaiol. Profiling of multiple cannabis flower samples detected over 15 terpenes above 5 ppm, including key compounds such as limonene, γ-terpinene, terpineol, β-caryophyllene, (–)-isopulegol, (+)-cedrol, and (–)-α-bisabolol. Representative chromatograms confirmed retention times and spectral purity for each analyte.

Benefits and practical applications

• Solvent-free extraction reducing consumable costs and environmental impact
• Cleaner spectra through limited matrix interference
• Rapid analysis with total cycle time under 30 minutes for high throughput
• Spectral confirmation enhances confidence in compound identification

Future trends and opportunities

With further validation and calibration, this SPME headspace approach can be extended to routine quantitative terpene testing in cannabis and hemp matrices. Advances in SPME Arrow technology promise increased phase volume for trace-level detection. Integration with automation and high-resolution MS will broaden applications to food quality, environmental monitoring, and pharmaceutical analysis.

Conclusion

This study establishes a fast, reproducible, and solvent-free SPME-GC/MS method using a DVB/CAR/PDMS fiber for terpene profiling in cannabis flower. As a proof of principle, the method demonstrates strong potential for adoption in research and quality control settings following further method development.

References

1. Agilent Technologies. SPME Arrow Sampling of Terpenes in Cannabis Plant Material. Application Note 5994-1046EN, 2019.
2. Greencamp. 15 Terpenes in Cannabis Explained. Cannacon, 2019.
3. Potbotics. Terpenes: Isopulegol. Potbotics, 2019.
4. The Apothecarium. Terpenes the Essentials: Isopulegol. The Apothecarium, 2018.
5. Kagawa D., et al. The Sedative Effects and Mechanism of Action of Cedrol Inhalation with Behavioral Pharmacological Evaluation. Planta Medica 69(7):637–641, 2003.