title: Development and validation of a liquid chromatography-tandem mass spectrometric assay for quantitative analyses of triptans in hair.
abstract: 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.
authors.affiliation: 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. Electronic address: daniele.vandelli@unimore.it.
authors.forename: Daniele
authors.initials: D
authors.lastname: Vandelli
authors.affiliation: 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.
authors.forename: Federica
authors.initials: F
authors.lastname: Palazzoli
authors.affiliation: 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.
authors.forename: Patrizia
authors.initials: P
authors.lastname: Verri
authors.affiliation: Department of Life Sciences, University of Modena and Reggio Emilia, via G. Campi, 103, 41125 Modena, Italy.
authors.forename: Cecilia
authors.initials: C
authors.lastname: Rustichelli
authors.affiliation: 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.
authors.forename: Filippo
authors.initials: F
authors.lastname: Marchesi
authors.affiliation: Department of Diagnostic, Clinical and Public Health Medicine, Unit of Medical Toxicology, Headache and Drug Abuse Centre, University of Modena and Reggio Emilia, via del Pozzo, 71, 41124 Modena, Italy.
authors.forename: Anna
authors.initials: A
authors.lastname: Ferrari
authors.affiliation: Department of Diagnostic, Clinical and Public Health Medicine, Unit of Medical Toxicology, Headache and Drug Abuse Centre, University of Modena and Reggio Emilia, via del Pozzo, 71, 41124 Modena, Italy.
authors.forename: Carlo
authors.initials: C
authors.lastname: Baraldi
authors.affiliation: Clinical and Experimental Medicine Doctorate School, University of Modena and Reggio Emilia, via del Pozzo, 71, 41124 Modena, Italy.
authors.forename: Enrico
authors.initials: E
authors.lastname: Giuliani
authors.affiliation: 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.
authors.forename: Manuela
authors.initials: M
authors.lastname: Licata
authors.affiliation: 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.
authors.forename: Enrico
authors.initials: E
authors.lastname: Silingardi
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D006197:Hair / Q000737:chemistry*; D006801:Humans; D057230:Limit of Detection; D012015:Reference Standards; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014363:Tryptamines / Q000032:analysis*
chemical_list: D014363:Tryptamines
keywords: HPLC–MS/MS; Hair samples; Migraine; Overuse; Triptans