Residual Solvents in Cannabis Concentrates on Rxi®-624Sil MS by Headspace–Full Evaporation Technique (HS-FET)

PeakstR (min)
1.Isobutane0.910
2.Butane0.996
3.Methanol1.112
4.Pentane1.508
5.Ethanol1.545
6.Acetone1.795
7.Isopropanol1.891
8.n-Hexane2.412
9.Chloroform2.962
10.Benzene3.213
11.Heptane3.363
12.Toluene4.135
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GC_FS0517
ColumnRxi®-624Sil MS, 30 m, 0.25 mm ID, 1.40 µm (cat.# 13868)
SampleResidual solvent mix
Diluent:Dimethyl sulfoxide (DMSO)
Conc.:500 ppm (For the HS-FET technique, 10 µL of a 1,000 µg/mL standard was placed into a 20 mL headspace vial to represent a 500 ppm sample concentration, assuming a 20 mg sample.)
Injectionheadspace-loop split (split ratio 10:1)
Liner:Premium 1.0 mm ID straight inlet liner (cat.# 23333.1)
Headspace-Loop
Inj. Port Temp.:250 °C
Instrument:Tekmar HT3
Inj. Time:1.0 min
Transfer Line Temp.:160 °C
Valve Oven Temp.:160 °C
Needle Temp.:140 °C
Sample Temp.:140 °C
Platen temp equil. time:1.0 min
Sample Equil. Time:30.0 min
Vial Pressure:20 psi
Pressurize Time:5.0 min
Loop Pressure:15 psi
Loop Fill Time:2.0 min
Oven
Oven Temp.:35 °C (hold 1.5 min) to 300 °C at 30 °C/min (hold 2.0 min)
Carrier GasHe, constant flow
Linear Velocity:80 cm/sec
DetectorFID @ 250 °C
Make-up Gas Flow Rate:45 mL/min
Make-up Gas Type:N2
Hydrogen flow:40 mL/min
Air flow:450 mL/min
Data Rate:20 Hz
InstrumentAgilent/HP6890 GC
NotesThe FID temperature in this chromatogram was set too low in error. FID temperature should be set to 320°C for residual solvent analysis. This will not affect peak shape or elution profile, but will ensure terpenes do not condense on FID jet.

The butane used for standard preparation was a mixture of butane and isobutane in an unknown ratio. The concentrations of butane and isobutane should be considered approximate, but do not exceed 500 ppm for either component.
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