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

Column | Rxi-624Sil MS, 30 m, 0.25 mm ID, 1.40 µm (cat.# 13868) |
Sample | Residual 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.) |
Injection | headspace-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 Gas | He, constant flow |
Linear Velocity: | 80 cm/sec |
Detector | FID @ 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 |
Instrument | Agilent/HP6890 GC |
Notes | The 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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