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Under Pressure? Low-Pressure Gas Chromatography Analysis of Cannabinoid Neutrals

01 Aug 2024

Cannabinoid neutrals are a group of chemical compounds naturally produced by cannabis plants. They are primarily found in the resin produced by the flowers and leaves of the cannabis plant. Some of the most well-known neutrals include delta-8- and delta-9-tetrahydrocannabinol (THC) and cannabidiol (CBD). Respectively, these compounds are known for the psychoactive effects of cannabis and the potential for therapeutic uses.

Figure 1: Cannabinoid Neutrals 9 Standard on LPGC Rxi-35Sil MS
Cannabinoid Neutrals 9 Standard on LPGC Rxi-35Sil MS

GC_GN1243

Peaks

PeakstR (min)Conc.
(…)
1.Cannabidivarin4.75320
2.Tetrahydrocannabivarin5.01320
3.Cannabicyclol5.05720
4.Cannabichromene5.14220
5.Cannabidiol5.18920
6.d8-Tetrahydrocannabinol5.36720
7.d9-Tetrahydrocannabinol5.43320
8.Cannabigerol5.48720
9.Cannabinol5.59020

Conditions

ColumnLPGC Rxi-35Sil MS, includes Rxi-35mSil MS 10 m 0.32 mm 0.25 µm w/ 5 0.15 mm ID Rxi restrictor connected via SilTite connector
Standard/SampleCannabinoids Neutrals 9 Standard (cat.# 34132)
Diluent:Methanol
Conc.:100 µg/mL (20 µg/mL on column)
Injection
Inj. Vol.:1 µL split (split ratio 5:1)
Liner:Topaz, splitless, single taper inlet liner, 4.0 mm x 6.5 x 78.5 (cat.# 23303)
Inj. Temp.:290 °C
Split Vent Flow Rate:4.5 mL/min
Oven
Oven Temp.:80 °C to 300 °C at 40 °C/min (hold 1 min)
Carrier GasHe, constant flow
Flow Rate:0.9 mL/min
DetectorMS
Mode:Scan
Scan Program:
GroupStart Time
(min)
Scan Range
(amu)
Scan Rate
(scans/sec)
11.530-5505.3
Transfer Line Temp.:300 °C
Analyzer Type:Quadrupole
Source Temp.:330 °C
Quad Temp.:180 °C
Solvent Delay Time:1.5 min
Tune Type:PFTBA
Ionization Mode:EI
InstrumentAgilent 7890A GC & 5975C MSD
Sample PreparationThe sample was in a 2 mL short-cap, screw-thread vial (cat.# 21143) and capped with a short-cap, screw-vial closure (cat.# 24495).

This analysis was completed using low pressure gas chromatography mass spectrometry (LPGC GC-MS). LPGC is a great technique to pair with a mass spectrometer detector in the confirmation and identification of various compounds. LPGC uses a deactivated microbore column joined via a connector to a medium bore or megabore analytical column. With fast temperature programming and reduced flow rates, LPGC allows for increased optimum linear velocity.  Using this technique can result in faster GC run times, increased sensitivity, and taller, narrower peaks.

The cannabinoid neutrals standard was run on an LPGC kit consisting of an Rxi-35Sil MS analytical column (10 m × 0.32 mm × 0.25 µm) with a 5 m × 0.15 mm ID Rxi restrictor connected via SilTite connector. The Rxi-35Sil MS is an excellent choice for cannabinoid analysis due to its selectivity and increased thermal stability. It is also compatible with a diverse range of analytes, including polar and nonpolar compounds, making it versatile for different analytical applications.

The image below shows the difference between a conventional GC-MS (black) analysis of cannabinoid neutrals and the LPGC (red) analysis. By using LPGC, the first eluting compound—cannabidivarin (CBDV)—comes out six minutes sooner than the conventional analysis times. Run times are reduced to six minutes with LPGC as the last compound—cannabinol (CBN)—measured against the thirteen minutes needed for a regular GC analysis. Despite the reduced separation efficiency, LPGC was able to provide satisfactory resolution for these analytes.

figure blog jessi LPGC comparison 1
Cannabinoid Neutrals 
Number Compound LPGC-MS RT Conventional GC-MS RT Primary Ion(s) Resolution*
1 Cannabidivarin (CBDV) 4.753 11.06 203 8.29
2 Tetrahydrocannabivarin (THCV) 5.013 11.564 271 1.37
3 Cannabicyclol (CBL) 5.057 11.652 231 2.57
4 Cannabichromene (CBC) 5.142 11.793 231, 174 1.46
5 Cannabidiol (CBD) 5.189 11.9 231, 246 5.68
6 d8-Tetrahydrocannabinol (d8-THC) 5.367 12.248 231, 314 2.05
7 d9-Tetrahydrocannabinol (d9-THC) 5.433 12.373 299, 315 1.77
8 Cannabigerol (CBG) 5.487 12.451 193 3.28
9 Cannabinol (CBN) 5.590 12.677 295 5.60

*LPGC only. 

Related Products


Kit de colonnes GC basse pression (LPGC) Rxi-35Sil MS
Insert Topaz, Gooseneck Splitless, 4.0 mm x 6.5 x 78.5, pour GC Agilent, avec laine de quartz, désactivation Premium, lot de 5
Flacon à visser avec zone de marquage graduée, filetage 9 mm/425, 2.0 ml, 9 mm, 12 x 32 mm (flacon seulement), ambré, lot de 1000
Bouchon à filetage court, polypropylène, à visser, avec septum PTFE/silicone/PTFE, noir, assemblé, 2.0 ml, 9 mm, lot de 100
Cannabinoïdes 9 composés neutres, 1000 µg/ml, méthanol, ampoule de 1 ml

Author

  • Jessi Collier

    Jessi is an advanced scientist in the GC applications group where her work focuses on environmental and food contaminants. Prior to joining Restek in 2023, she worked for the Mississippi State Chemical Lab as a pesticide residue analyst, primarily testing regulatory samples, agricultural samples, environmental samples, foods, and other consumer products via GC-MS, GC-MS/MS, GC-FID, and GC-ECD. Jessi holds a BS in chemistry and a BA in Mandarin Chinese from Mississippi State University.

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