Vandelli Daniele, Palazzoli Federica, Verri Patrizia, Rustichelli Cecilia, Marchesi Filippo, Ferrari Anna, Baraldi Carlo, Giuliani Enrico, Licata Manuela, Silingardi Enrico
Department of Diagnostic Medicine, Clinical and Public Health, Unit of Legal Medicine-Forensic Toxicology Laboratory, University of Modena and Reggio Emilia, via del Pozzo, 71, 41124 Modena, Italy.
Department of Diagnostic Medicine, Clinical and Public Health, Unit of Legal Medicine-Forensic Toxicology Laboratory, University of Modena and Reggio Emilia, via del Pozzo, 71, 41124 Modena, Italy.
J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Apr 1;1017-1018:136-144. doi: 10.1016/j.jchromb.2016.02.031. Epub 2016 Feb 27.
Triptans are specific drugs widely used for acute treatment of migraine, being selective 5HT1B/1D receptor agonists. A proper assumption of triptans is very important for an effective treatment; nevertheless patients often underuse, misuse, overuse or use triptans inconsistently, i.e., not following the prescribed therapy. Drug analysis in hair can represent a powerful tool for monitoring the compliance of the patient to the therapy, since it can greatly increase the time-window of detection compared to analyses in biological fluids, such as plasma or urine. In the present study, a liquid chromatography-tandem mass spectrometric (LC-MS/MS) method has been developed and validated for the quantitative analysis in human hair of five triptans commonly prescribed in Italy: almotriptan (AL), eletriptan (EP), rizatriptan (RIZ), sumatriptan (SUM) and zolmitriptan (ZP). Hair samples were decontaminated and incubated overnight in diluted hydrochloric acid; the extracts were purified by mixed-mode SPE cartridges and analyzed by LC-MS/MS under gradient elution in positive multiple reaction monitoring (MRM) mode. The procedure was fully validated in terms of selectivity, linearity, limit of detection (LOD) and lower limit of quantitation (LLOQ), accuracy, precision, carry-over, recovery, matrix effect and dilution integrity. The method was linear in the range 10-1000pg/mg hair, with R(2) values of at least 0.990; the validated LLOQ values were in the range 5-7pg/mg hair. The method offered satisfactory precision (RSD <10%), accuracy (90-110%) and recovery (>85%) values. The validated procedure was applied on 147 authentic hair samples from subjects being treated in the Headache Centre of Modena University Hospital in order to verify the possibility of monitoring the corresponding hair levels for the taken triptans.
