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Extraction of THC and 11-Nor-Δ9-THC-Carboxylic Acid from Urine

Method:
Matrix
Application-No.:
SPE
urine
303880

Substances:THC; THC-COOH; 11-Nor-Δ9-THC-Carboxylic Acid
Column:CHROMABOND® Drug II, 3 ml, 200 mg
Phase:CHROMABOND Drug II
MN catalog number:730680
Sample pretreatment:To 5 ml urine 300 μl 10 M potassium hydroxide solution and internal standard (for GC-MS deuterium labeled 11-nor-Δ9-THC-carboxylic acid) are added. The sample is vortexed and then hydrolysed at 60 °C for 15 min. The sample is cooled and 200 μl glacial acetic acid and 2 ml 50 mM ammonium acetate solution are added. If necessary the sample pH is adjusted to 6.0 – 7.0.
Conditions:Column conditioning: 2 ml methanol, followed by 2 ml distilled water – equilibrate column with 2 ml 50 mM ammonium acetate buffer

Sample application: slowly force or aspirate the sample through the column (1-2 ml per min)

Column washing: interferences are eluted with 10 ml methanol – water (1:1, v/v); the column is dried for 10 min at high vacuum; the column is further washed with 2 ml acetonitrile and dried for another 2 min

Elution: THC metabolites are eluted with 3 ml hexane – ethyl acetate – glacial acetic acid (75:25:1, v/v/v)
Detection
Subsequent analysis:
For further analysis we recommend GC-MS on an OPTIMA® 5 MS (e.g. Cat. No. 726220.30) column after derivatisation with 50 μl Silyl-991 (Cat. No. 701480; BSTFA –TMCS 99:1) at 70°C / 20 min – inject 1-2 μl onto GC.

Author(-s):SPE department
Source:MACHEREY-NAGEL; Germany; 2006

Keywords:drugs; THC; urine
Chromatogram:

Recovery rates: 70 - 80%
Legend:



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