Application of two-dimensional gas chromatography with electron capture chemical ionization mass spectrometry to the detection of 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) in hair.

The proposed federal regulations for the detection in hair of 11-nor-Delta(9)-tetrahydrocannabinol-9-carboxylic acid (THC-COOH), a metabolite of marijuana, require a confirmatory detection level of 0.05 pg/mg. At present, the only way to achieve this on a routine basis has been with the use gas chromatography with tandem mass spectrometry (GC-MS-MS) technology. Tandem MS is an expensive approach and dissuades laboratories from attempting to enter the hair-testing market. A procedure for the determination of THC-COOH in hair using two-dimensional gas chromatography (GC x GC) coupled to mass spectrometry (GC-GC-MS) is described for the first time. The method makes use of several small improvements in the extraction, GC, and MS procedures to allow the required sensitivity to be achieved. The results of this approach demonstrate detection of THC-COOH in hair at a concentration level of 0.05 pg/mg with both a target quantitation ion and a unique confirming qualifier ion, using a single-quadrupole mass selective detector. These two ions and the enhanced separation of the GC-GC provide a high degree of confidence in the determinations. The method has been successfully applied to the detection of THC-COOH in hair specimens from known marijuana users, and it reaches the levels currently proposed in the Federal Register.