Determination of delta 9-tetrahydrocannabinol-11-oic acid in urine as its pentafluoropropyl-pentafluoropropionyl derivative by GC/MS utilizing negative ion chemical ionization.
A rapid and sensitive GC/MS method for the determination of delta 9-tetrahydrocannabinol-11-oic acid in urine is presented. Enzymically hydrolyzed urine was extracted with hexane/ethyl ether followed by a one-step derivatization procedure with a mixture of pentafluoropropionic anhydride and pentafluoropropanol. By using negative ion chemical ionization and selected ion monitoring, a 200-fold higher detectability was observed, compared with El or positive ion chemical ionization under the conditions used. Samples were analyzed with split injection on a fused silica capillary column with a total analysis time of less than four minutes. A deuterium labelled analogue was used as internal standard and the precision for the overall method was measured to 3.4% for a sample concentration of 230 ng/mL, and to 6.7% for 3 ng/mL. The minimum detectable amount was below 1 ng/mL.
D055598:Chemical Phenomena; D002621:Chemistry; D013759:Dronabinol / Q000031:analogs & derivatives* / Q000652:urine; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006801:Humans; D006868:Hydrolysis
C016780:11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic acid; D013759:Dronabinol