Development and validation of a liquid chromatography-tandem mass spectrometric assay for quantitative analyses of triptans in hair

作者：Vandelli Daniele^*; Palazzoli Federica; Verri Patrizia; Rustichelli Cecilia; Marchesi Filippo; Ferrari Anna; Baraldi Carlo; Giuliani Enrico; Licata Manuela; Silingardi Enrico

来源：Journal of Chromatography B-Analytical Technologies in the Biomedical and Life Sciences, 2016, 1017: 136-144.

DOI：10.1016/j.jchromb.2016.02.031

• Triptans
• HPLC-MS/MS
• Hair samples
• Migraine
• Overuse

Triptans are specific drugs widely used for acute treatment of migraine, being selective 5HT(1B/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 10-1000 pg/mg hair, with R-2 values of at least 0.990; the validated LLOQ values were in the range 5-7 pg/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.

• 出版日期2016-4-1