Ultrasensitive analysis of lysergic acid diethylamide and its C-8 isomer in hair by capillary zone electrophoresis in combination with a stacking technique and laser induced fluorescence detection

• New method based on CZE-LIF to monitor LSD and iso-LSD in hair.
• FASI used as on-line sample preconcentration technique for enhancing sensitivity.
• Ultrasound assisted solid–liquid extraction employed for drug extraction from the hair.
• Detection limits (3 S/N) around 0.100 pg mg−1 with RSD lower than 10%.
• Recoveries of 73.3 and 79.9% for LSD and iso-LSD, respectively.

This article deals with the development and validation of a novel capillary zone electrophoresis (CZE) with laser induced fluorescence detection method for the analysis of lysergic acid diethylamide (LSD) and its isomer iso-LSD in hair samples. The separation of both analytes has been achieved in less than 13 min in a 72-cm effective length capillary with 75-μm internal diameter. As running buffer 25 mM citrate, pH 6.0 has been employed and separation temperature and voltage of 20 °C and 13 kV respectively, were applied. Field amplified sample injection (FASI) has been employed for on-line sample preconcentration, using ultrapure water containing 117 μM H3PO4 as optimum injection medium. Injection voltage and time have been optimized by means of experimental design, obtaining values of 7 kV and 15 s, respectively. Methylergonovine has been employed as internal standard in order to compensate irreproducibility from electrokinetic injection. The analytical method has been applied to hair samples, previous extraction of the target analytes by ultrasound assisted solid–liquid extraction at 40 °C for 2.5 h, employing acetonitrile as extracting solvent. Linear responses were found for LSD and iso-LSD in matrix-matched calibrations from around 0.400 up to 50.0 pg mg−1. LODs (3 S/N) in the order of 0.100 pg mg−1 were calculated for both analytes, obtaining satisfactory recovery percentages for this kind of sample.

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