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GC/MS Analysis of Terpenes

HPLC/MS and GC/MS can both be used for the quantification of various terpenes found within C. sativa cultivars. The choice of HPLC/MS is, however, more ideal for the sake of simplicity, as using a single column shared between cannabinoid quantification, residual pesticide analysis, and terpene quantification ensure simplicity and fast analyses. To the right is a list, taken from here, depicting a list of possible terpenes and their corresponding Certified Reference Materials available from Sigma-Aldrich. 

GC/MS Terpene Quantification Standards

Standard solutions of terpene certified reference materials created as follows;

  • In a single vial, create a solution in ethyl acetate of 1.0mg/mL each of:

    • α​-pinene

    • (-)-β-pinene

    • Myrcene

    • R-t-limonene

    • Terpinolene

    • Linalool

    • α​-terpeneol

    • β-caryophyllene

    • α​-humulene

    • Caryophyllene oxide

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Calibration Curve

  • The standard solution was serial diluted and adjusted with the internal standard to contain 100μg/mL of n-tridecane

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Internal standard

  • To each calibration and sample solution, add 100μg/mL of n-tridecane, adjusted for maintaining the concentration of the calibration solutions. 

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Sample Preparation

  • For flower samples: Samples are to be dried for 24h at 40℃ then ground to a powder 

    • Samples of 1.0g each, in triplicate, are extracted in 10mL of extraction solution

      • ​100​μg/mL in ethyl acetate

      • Extracted by sonication for 10min

    • Centrifuge flower extract at 1252 x g for 5 minutes and transfer supernatant to a new tube

  • For oil samples: Samples of 1.0g oil each, in triplicate, are dissolved in 10mL of extraction solution, outlined above

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GC/MS Terpene Analysis Conditions

All conditions outlined here were taken in a digested format from Ibrahim et al., 2019, (DOI: 10.1055/a-0828-8387) which can be found here.

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Instruments:

  • GC: Agilent 7890A Series

    • MS: Agilent 5975C MDS

    • ALS: Agilent 7693 (optional)​

    • HS: Agilent

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Gas Chromatography Conditions:

  • Column: DB-5MS Capillary Column (30 m × 0.25 mm I. D., 0.25 µm particle size)

  • Carrier gas: Helium

    • Flow: constant, 1mL/min​

  • Inlet Temperature: 250℃ 

  • Split ratio: 15:1

  • Injection volume: 2μL 

  • Temperature program:

    • 50​℃ - 2 min

    • Ramp 2℃/min to 85℃ 

    • Ramp 3℃/min to 165℃ 

    • Clearing post run - 280℃ - 10 min

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Mass Spectrophotometer Conditions:

  • Mode: Full Scan

  • Range: 40-450 amu

  • Ionization energy: 70eV

  • Ion source temperature: 230℃ 

  • Quadrupole temperature: 150℃ 

  • Solvent delay: 4 min

  • Software assisted compound identification: NIST

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