Determination of different recreational drugs in hair by HS-SPME and GC/MS

• Published in: Analytical and bioanalytical chemistry Vol. 397; no. 7; pp. 2987 - 2995
• Main Authors: Merola, Gustavo, Gentili, Stefano, Tagliaro, Franco, Macchia, Teodora
• Format: Journal Article
• Language: English
• Published: Berlin/Heidelberg Berlin/Heidelberg : Springer-Verlag 01.08.2010; Springer-Verlag; Springer
• Subjects: amphetamines; Analysis; Analytical Chemistry; Biochemistry; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Chromatographic methods and physical methods associated with chromatography; Chromatography; Cocaine; Drugs; Exact sciences and technology; Food Science; Gas chromatographic methods; Gas Chromatography-Mass Spectrometry - methods; Hair; Hair - chemistry; Hallucinogenic drugs; Headspace solid-phase microextraction and gas chromatography-mass spectrometry; Humans; Hydrolysis; ketamine; Laboratory Medicine; Limit of Detection; Mass spectrometry; Mathematical analysis; Monitoring/Environmental Analysis; Original Paper; Solid Phase Microextraction - methods; Spectrometric and optical methods; Street Drugs - analysis; Substance Abuse Detection - methods; Tetrahydrocannabinol; Hair; Headspace solid-phase microextraction and gas chromatography–mass spectrometry; Ketamine; ∆; Amphetamines; Cocaine; Tetrahydrocannabinol; Microanalysis; Derivatization; Chemical enrichment; Accuracy; Δ; Detection limit; Headspace solid-phase microextraction and gas chromatography-mass spectrometry; Amfetamine; Variation coefficient; Drug; Sample; Use; Solid phase microextraction; Gas chromatography; Repeatability; Adsorption; Linearity; Quality control; Simultaneous measurement; Alkaline hydrolysis; Headspace; Parameter; Application; Mass spectrometry
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-010-3882-6

A simple procedure combining headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC/MS) to detect and quantify amphetamines, ketamine, methadone, cocaine, cocaethylene and ∆⁹-tetrahydrocannabinol (THC) in hair is described. This procedure allows, in a single sample, even scant, analysis of drugs requiring different analytical conditions. A hair sample (10 mg) is washed and subjected to acidic hydrolysis. Then the HS-SPME is carried out (10 min at 90 °C) for amphetamines, ketamine, methadone, cocaine and cocaethylene. For derivatization of analytes, the fibre is introduced into the headspace of another closed vial containing acetic anhydride. After a chromatographic run, an alkaline hydrolysis for THC analysis is carried out in the same vial containing the hair sample previously used. For adsorption, the solid-phase microextraction needle is inserted into the headspace of the vial and the fibre is exposed for 30 min at 150 °C. For derivatization of analytes, the fibre is introduced into the headspace of another closed vial containing N-methyl-N-(trimethylsilyl)trifluoroacetamide. The GC/MS parameters were the same for both chromatographic runs. The linearity was proved to be between 0.01 and 10.00 ng/mg. The repeatability (intra- and interday precision) was below 10% as the coefficient of variation for all compounds. The accuracy, as the relative recovery, was 96.2-103.5% (spiked samples) and 88.6-101.7% (quality control sample). The limit of detection ranged from 0.01 to 0.12 ng/mg, and the limit of quantification ranged from 0.02 to 0.37 ng/mg. Application of the procedure to real hair samples is described. To the best of our knowledge, the proposed procedure combining HS-SPME and GC/MS is the first one be to successfully applied to the simultaneous determination of most of the common recreational drugs, including THC, in a single hair sample.