Sample preparation for GC-MS analysis

1.

Prepare a standard curve each time samples are being analyzed. Set up 9 tubes
containing 1ml of methanol and the following:

Tube 1
Tube 2
Tube 3
Tube 4
Tube 5
Tube 6
Tube 7
Tube 8
Tube 9

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Spike 1: 12L
Spike 2: 30L
Spike 3: 60L
Spike 4: 120L
Spike 5: 300L
Spike 6: 600L
Spike 7: 1.2mL
LQ: 48L
HQ: 48L

(0.05 mg/L)
(0.125mg/L)
(0.250mg/L)
(0.5mg/L)
(1.25mg/L)
(2.50mg/L)
(5mg/L)
(0.20mg/L From a 0.5mg/L LQ stock)
(4mg/L - From a 10mg/L HQ stock)

Note: All volumes of THC used come from a standard stock with a concentration of
0.5mg/L (Please refer to appendix for making the THC stock).
2.

Add 200L of the internal standard to all tubes. Vortex all tubes and centrifuge
them at 43C for 1hr.

3.

Make up a mixture of Hexane:BSTFA (4:1) and add 120L to all tube. Vortex and
cap all tubes.

4.

Incubate all tubes for 20 minutes in a 70C oil bath and then allow the samples to
cool down at 4C for 5 minutes.

5.

Transfer all the samples to GC analysis vials and load them onto the GC-MS.

Appendix
Before each analysis, the following must be available:
1. 0.5mg/L stock of THC and 0.5mg/L stock of D3 THC (internal std). To make up
stock add 50L of THC or D3 THC into 9.95mL of methanol.
2. 0.5mg/L LQ and 10mg/L HQ stock of THC which is to be made up in methanol
and water (1:1).
3. Hexane, Methanol (both being HPLC grade) and BSTFA.