title: Analysis of synthetic cannabinoids in herbal blends by means of nano-liquid chromatography.
abstract: In this study, a rapid and simultaneous separation of 12 synthetic cannabinoids and Δ(9)-tetrahydrocannabinol (Δ(9)-THC) in herbal blends was obtained by means of nano-liquid chromatography (nano-LC). The nano-LC experiments were performed in a 100μm i.d. capillary column packed with Cogent(®) bidentate C(18) silica particles for 25.0cm. All compounds were resolved using an isocratic elution mode in less than 30min. A mobile phase containing ACN/MeOH/H(2)O/formic acid 69/5/25/1 (v/v/v/v) was employed for the chromatographic separation. The developed analytical method was validated in terms of precision, linearity, sensitivity and accuracy. Under optimal nano-LC-UV conditions, the resulting RSD percentages for intra-day and inter-day repeatability, related to retention time and peak area, were below 2.98 and 6.40%, respectively. Limits of detection and quantification were 0.2 and 0.5μg/mL, respectively, for all the studied compounds. Linearity was assessed in the concentration range of interest for all analytes with determination coefficients r(2)≥0.9975. The method was then applied to the determination of synthetic cannabinoids in herbal blends. Quantitative analyses of the cannabimimetic compounds in six products showed that there was a wide difference in the concentration of the studied compounds among different products. Further, the nano-LC system was coupled with a mass spectrometer measuring the MS and MS-MS spectra to unequivocally identify the cannabinoids present in smoking mixtures.
authors.affiliation: Department of Therapeutic Research and Medicines Evaluation, Istituto Superiore di Sanità, Viale Regina Elena 299, Rome 00161, Italy.
authors.forename: Gustavo
authors.initials: G
authors.lastname: Merola
authors.forename: Zeineb
authors.initials: Z
authors.lastname: Aturki
authors.forename: Giovanni
authors.initials: G
authors.lastname: D'Orazio
authors.forename: Rossella
authors.initials: R
authors.lastname: Gottardo
authors.forename: Teodora
authors.initials: T
authors.lastname: Macchia
authors.forename: Franco
authors.initials: F
authors.lastname: Tagliaro
authors.forename: Salvatore
authors.initials: S
authors.lastname: Fanali
mesh_terms: D002186:Cannabinoids / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D013759:Dronabinol / Q000032:analysis; D013058:Mass Spectrometry / Q000379:methods; D036103:Nanotechnology / Q000379:methods; D028321:Plant Preparations / Q000737:chemistry*; D012680:Sensitivity and Specificity; D012822:Silicon Dioxide / Q000737:chemistry
chemical_list: D002186:Cannabinoids; D028321:Plant Preparations; D012822:Silicon Dioxide; D013759:Dronabinol