Licata Manuela, Rustichelli Cecilia, Palazzoli Federica, Ferrari Anna, Baraldi Carlo, Vandelli Daniele, Verri Patrizia, Marchesi Filippo, Silingardi Enrico
Department of Diagnostic Medicine, Clinical and Public Health, Division of Legal Medicine, University of Modena and Reggio Emilia, Via del Pozzo 71, 41124 Modena, Italy.
Department of Life Sciences, University of Modena and Reggio Emilia, Via G. Campi, 103, 41125 Modena, Italy.
J Pharm Biomed Anal. 2016 Jul 15;126:14-25. doi: 10.1016/j.jpba.2016.04.015. Epub 2016 Apr 14.
Headache patients suffering from recurrent attacks are a population at risk of overuse and abuse of analgesic medications. Associated with triptans, the first-line drugs recommended for the acute treatment, these patients usually take other medications such as opioids analgesics for the attack treatment, antidepressants and antiepileptics for prophylaxis treatment and benzodiazepines, non-benzodiazepine hypnotics and antipsychotics for the treatment of comorbidities. Regular and frequent use of triptans, like of any other symptomatic analgesic, can cause chronic headache and medication-overuse headache (MOH). In these circumstances, a detoxification treatment is necessary and therefore the monitoring and follow-up of the patients are crucial to the success of the treatment. In the present study, a LC tandem MS method has been developed for the identification of 50 psychoactive drugs in human hair, including triptans, benzodiazepines and metabolites, analgesics, antiepileptic, antidepressants and metabolites, a non-benzodiazepine hypnotic (z-drug), antipsychotics and metabolites. Hair samples were decontaminated, pulverized and incubated overnight in methanol; the extracts were then purified by a new and rapid QuEChERS procedure and analyzed by LC-MS/MS under gradient elution with positive ionization MRM mode. The procedure was fully validated in terms of selectivity, linearity, limit of detection and lower limit of quantitation, precision and accuracy, carry-over, matrix effect, recovery and dilution integrity. The validated procedure has been applied to 234 real hair samples collected from headache patients with known type and dosage of the taken drugs; the obtained data could be of interest to evaluate the xenobiotic concentrations in patients with known therapy.
患有反复发作性头痛的患者是存在过度使用和滥用止痛药物风险的人群。与曲坦类药物相关，这些药物是推荐用于急性治疗的一线药物，这些患者通常会服用其他药物，如用于发作治疗的阿片类镇痛药、用于预防治疗的抗抑郁药和抗癫痫药，以及用于治疗合并症的苯二氮䓬类药物、非苯二氮䓬类催眠药和抗精神病药。像其他任何对症镇痛药一样，经常规律使用曲坦类药物会导致慢性头痛和药物过量使用性头痛（MOH）。在这些情况下，排毒治疗是必要的，因此对患者的监测和随访对于治疗的成功至关重要。在本研究中，开发了一种液相色谱串联质谱法，用于鉴定人发中的50种精神活性药物，包括曲坦类药物、苯二氮䓬类药物及其代谢物、镇痛药、抗癫痫药、抗抑郁药及其代谢物、一种非苯二氮䓬类催眠药（Z类药物）、抗精神病药及其代谢物。头发样本经过去污、粉碎并在甲醇中孵育过夜；然后通过一种新的快速QuEChERS方法对提取物进行纯化，并在正离子MRM模式下的梯度洗脱条件下通过液相色谱-质谱/质谱进行分析。该方法在选择性、线性、检测限和定量下限、精密度和准确度、残留、基质效应、回收率和稀释完整性方面进行了全面验证。经过验证的方法已应用于从已知所服用药物类型和剂量的头痛患者中收集的234份真实头发样本；所获得的数据可能有助于评估已知治疗患者体内的外源性物质浓度。
