Quantitative GG-MS analysis of Delta(9)-tetrahydrocannabinol in fiber hemp varieties

A sensitive and specific method for the determination of total available Δ-tetrahydrocannabinol in fiber hemp varieties is described. The method was used for the regulatory purposes in which the detection of higher than the maximum allowed concentration of the psychoactive cannabinoid, Δ-tetrahydrocannabinol, in industrial fiber hemp would result in cancellation of the grower's license. Cannabinoids were extracted from dry leaf powder into hexane containing internal standard chrysene-d using sonication. Δ-Tetrahydrocannabinol in the extract was separated by gas chromatography and quantitated by mass spectroscopy. A linear calibration range extending to 40 ppm and a limit of detection of 0.2 ng were obtained by using the total ion current mode of detection

Shortcomings of protein removal prior to high performance liquid chromatographic analysis - A case study using method development for BAY 11-7082

During the analytical method development for BAY 11-7082 ((E)-3-[4-methylphenylsulfonyl]-2-propenenitrile), using HPLC-MS-MS and HPLC-UV, we observed that the protein removal process (both ultrafiltration and precipitation method using organic solvents) prior to HPLC brought about a significant reduction in the concentration of this compound. The use of a structurally similar internal standard, BAY 11-7085 ((E)-3-[4-t-butylphenylsulfonyl]-2-propenenitrile), was not effective in compensating for the loss of analyte as the extent of reduction was different to that of the analyte. We present here a systematic investigation of this problem and a new validated method for the determination of BAY 11-7082. (c) 2006 Elsevier B.V. All rights reserved