title: Hollow fiber-based liquid phase microextraction with factorial design optimization and gas chromatography-tandem mass spectrometry for determination of cannabinoids in human hair.
abstract: A new method, based on hollow fiber liquid-phase microextraction (HF-LPME) and gas chromatography-tandem mass spectrometry (GC-MSMS), was developed for determination of Delta(9)-tetrahydrocannabinol (THC), cannabidiol (CBD) and cannabinol (CBN) in samples of human hair. Since hair is a solid matrix, the samples were subjected to alkaline digestion using NaOH. The aqueous solutions obtained were extracted using a 6cm polypropylene fiber (600microm i.d., 200microm wall thickness, 0.2microm pore size) for each extraction. A 2(5-1) fractional factorial design for screening, and a central composite design for optimization of significant variables, was applied during development of the extraction method. The variables evaluated were the type of extraction solvent, pH, stirring speed, extraction time, and acceptor phase volume. The optimized conditions for the proposed extraction procedure were 10mg of hair sample; 20microL of butyl acetate; aqueous (pH 14) donor phase containing 6.8% NaCl; 600rpm stirring speed; 20min extraction time. A linear response was obtained in the ranges 1-500pgmg(-1) (CBD and CBN) and 20-500pgmg(-1) (THC), with regression coefficients >0.99. Precision, determined as the relative standard deviation, was 3.3-8.9% (intra-day) and 4.4-13.7% (inter-day). Absolute recoveries varied in the ranges 4.4-4.8% (CBD), 7.6-8.9% (THC) and 7.7-8.2% (CBN). Limits of detection (LOD, S/N=3) and quantification (LOQ, S/N=10) were 0.5-15pgmg(-1) and 1-20pgmg(-1), respectively. The method was successfully used to determine CBD, THC and CBN in hair samples from patients in a drug dependency rehabilitation center. Concentrations varied in the ranges 1-18pgmg(-1) (CBD), 20-232pgmg(-1) (THC) and 9-107pgmg(-1) (CBN), confirming the suitability of the method for monitoring studies.
authors.affiliation: Laboratório de Análise de Compostos Orgânicos Poluentes, Departamento de Química, Universidade Federal de Sergipe, Av. Marechal Rondon, s/n., Jardim Rosa Elze, 49100-000 São Cristóvão, SE, Brazil.
authors.forename: Elissandro Soares
authors.initials: ES
authors.lastname: Emídio
authors.forename: Vanessa
authors.initials: V
authors.lastname: de Menezes Prata
authors.forename: Fernando José Malagueño
authors.initials: FJ
authors.lastname: de Santana
authors.forename: Haroldo Silveira
authors.initials: HS
authors.lastname: Dórea
mesh_terms: D000704:Analysis of Variance; D002186:Cannabinoids / Q000032:analysis*; D005591:Chemical Fractionation / Q000295:instrumentation / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006197:Hair / Q000737:chemistry*; D006801:Humans; D006863:Hydrogen-Ion Concentration; D016014:Linear Models; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012997:Solvents; D015813:Substance Abuse Detection; D019966:Substance-Related Disorders / Q000534:rehabilitation; D053719:Tandem Mass Spectrometry
chemical_list: D002186:Cannabinoids; D012997:Solvents