In this study, a rapid chiral separation of 12 cathinones analogs has been developed and validated using cyclodextrin-assisted CE with UV and TOF-MS detection. Optimum separation was obtained on a 57.5 cm × 50 μm capillary using a buffer system consisting of 10 mM β-cyclodextrin (β-CD) in a 100 mM phosphate buffer for CE-UV, and 0.6% v/v highly sulfated-γ-cyclodextrin (HS-γ-CD) in a 50 mM phosphate buffer for CE-MS. In the CE-MS experiment, a partial filling technique was employed to ensure that a minimum amount of cyclodextrin entered the mass spectrometer. All analytes were separated within 18 min in the CE-UV separation and identified by TOF-MS. Ten compounds were enantiomerically separated using β-CD in the UV mode and an additional two more were enantiomerically separated using HS-γ-CD in the MS mode. Detection limits down to 1.0 ng/mL were obtained. The method was then applied to examine seized drugs.

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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 Delta(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 degrees 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 degrees 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.

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