Hair testing in clinical setting: Simultaneous determination of 50 psychoactive drugs and metabolites in headache patients by LC tandem MS

Licata, Manuela; Rustichelli, Cecilia; Palazzoli, Federica; Ferrari, Anna; Baraldi, Carlo; Vandelli, Daniele; Verri, Patrizia; Marchesi, Filippo; Silingardi, Enrico

doi:10.1016/j.jpba.2016.04.015

Cited by 48 publications

(30 citation statements)

References 37 publications

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“…The concentrations of sertraline, in this case, were in line with those found previously in two volunteers undergoing treatment with sertraline (50 mg/day), whose sertraline concentrations in hair were measured at 0.05 and 1.90 ng/mg . Higher concentrations in hair, at 0.44–55.9 ng/mg ( n = 9), have been reported in patients with known doses of sertraline . The doses in these publications were similar to or even lower than the doses administered in the present case (250–3000 mg/month vs 175–3900 mg/month).…”

Section: Resultssupporting

confidence: 92%

Segmental Hair Analysis—Interpretation of the Time of Drug Intake in Two Patients Undergoing Drug Treatment

Wang

Johansen

Nielsen

et al. 2018

Journal of Forensic Sciences

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The present study involved segmental testing of hair in two clinical cases with known dosage histories. Hair analysis confirmed the first patient's exposure to the prescribed sertraline and citalopram for several months. Citalopram was generally distributed along the hair shaft in accordance with the drug ingestion period. By contrast, “false” positive results were observed for sertraline in distal hair segments, corresponding to a period of no sertraline exposure, which may indicate incorporation from sweat or sebum, which transport the drugs along the hair surface. The second patient received various drugs during her treatment for brain cancer. Metoclopramide, morphine, oxazepam, paracetamol, sumatriptan, tramadol, and zopiclone, which had been part of the therapy, were all detected in the proximal hair segment. The results of these two cases indicated that results—especially concerning the time of drug intake—must be interpreted with caution and allow for the possibility of incorporation from sweat or sebum.

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Section: Resultssupporting

confidence: 92%

Segmental Hair Analysis—Interpretation of the Time of Drug Intake in Two Patients Undergoing Drug Treatment

Wang

Johansen

Nielsen

et al. 2018

Journal of Forensic Sciences

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“…However, a certain degree of nonadherence was present: nine samples were negative for the self-reported drug and nine were positive for unreported drugs. We hypothesized that these results depended on patients’ mistakes or forgetfulness rather than on shortcomings of the previously validated analytical method [12]. …”

Section: Discussionmentioning

confidence: 99%

“…The extraction and purification of the samples were performed according to Licata et al [12]. After decontamination and trituration, hair samples (50 mg aliquot) were added with 2.0 mL methanol and 20 μL of the IS solution and sonicated overnight at 45 °C; after addition of the roQ dSPE QuEChERS sorbent kit (2.0 mL, 150 mg MgSO4, 50 mg PSA-Primary Secondary Amine, 50 mg endcapped C18, Phenomenex, Torrance, CA, USA), the tubes were vortexed and centrifuged.…”

Section: Methodsmentioning

confidence: 99%

“…The purified hair extracts were then subjected to LC-MS/MS analysis (injection volume, 10 μL) on a Kinetex® Biphenyl column under the gradient elution conditions. The method had been developed by us and validated [12] according to the model proposed by the Scientific World Group for Forensic Toxicology in 2013, in standard practices for method validation in forensic toxicology [11]. Experimental details concerning LC-MS/MS analysis and method validation have been reported in a previous paper [12] and are briefly summarized as an online supplementary document.…”

Section: Methodsmentioning

confidence: 99%

“…Quantitative analyses of the drugs were performed on the basis of the calibration curves daily prepared and analyzed as reported [12]. …”

Section: Methodsmentioning

confidence: 99%

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Monitoring of adherence to headache treatments by means of hair analysis

Ferrari

Licata

Rustichelli

et al. 2016

Eur J Clin Pharmacol

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PurposeThe aim of this study was to evaluate the potential of hair analysis to monitor medication adherence in headache patients undergoing chronic therapy. For this purpose, the following parameters were analyzed: the detection rate of 23 therapeutic drugs in headache patients’ hair, the degree of agreement between the self-reported drug and the drug found in hair, and whether the levels found in hair reflected the drug intake reported by the patients.MethodsThe study included 93 patients suffering from primary headaches declaring their daily intake of at least one of the following drugs during the 3 months before the hair sampling: alprazolam, amitriptyline, citalopram, clomipramine, clonazepam, delorazepam, diazepam, duloxetine, fluoxetine, flurazepam, levomepromazine, levosulpiride, lorazepam, lormetazepam, mirtazapine, paroxetine, quetiapine, sertraline, topiramate, trazodone, triazolam, venlafaxine, and zolpidem.A detailed pharmacological history and a sample of hair were collected for each patient. Hair samples were analyzed by liquid chromatography-electrospray tandem mass spectrometry, using a previously developed method.ResultsAll 23 drugs were detected in the examined hair samples. The agreement between the self-reported drug and the drug found in hair was excellent for most analytes (P < 0.001, Cohen’s kappa); a statistically significant relationship (P < 0.05, linear regression analysis) between dose and hair level was found for amitriptyline, citalopram, delorazepam, duloxetine, lorazepam, and venlafaxine.ConclusionsHair analysis proved to be a unique matrix to document chronic drug use in headache patients, and the level found for each individual drug can represent a reliable marker of adherence to pharmacological treatments.Electronic supplementary materialThe online version of this article (doi:10.1007/s00228-016-2163-5) contains supplementary material, which is available to authorized users.

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Development and validation of an LC‐ESI‐MS/MS method for the quantification of D‐84, reboxetine and citalopram for their use in MS Binding Assays addressing the monoamine transporters hDAT, hSERT and hNET

Neiens

Simone

Ramershoven

et al. 2018

Biomedical Chromatography

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MS Binding Assays represent a label-free alternative to radioligand binding assays. In this study, we present an LC-ESI-MS/MS method for the quantification of (R,R)-4-(2-benzhydryloxyethyl)-1-(4-fluorobenzyl)piperidin-3-ol [(R,R)-D-84, (R,R)-1], (S,S)-reboxetine [(S,S)-2], and (S)-citalopram [(S)-3] employed as highly selective nonlabeled reporter ligands in MS Binding Assays addressing the dopamine [DAT, (R,R)-D-84], norepinephrine [NET, (S,S)-reboxetine] and serotonin transporter [SERT, (S)-citalopram], respectively. The developed LC-ESI-MS/MS method uses a pentafluorphenyl stationary phase in combination with a mobile phase composed of acetonitrile and ammonium formate buffer for chromatography and a triple quadrupole mass spectrometer in the multiple reaction monitoring mode for mass spectrometric detection. Quantification is based on deuterated derivatives of all three analytes serving as internal standards. The established LC-ESI-MS/MS method enables fast, robust, selective and highly sensitive quantification of all three reporter ligands in a single chromatographic run. The method was validated according to the Center for Drug Evaluation and Research (CDER) guideline for bioanalytical method validation regarding selectivity, accuracy, precision, calibration curve and sensitivity. Finally, filtration-based MS Binding Assays were performed for all three monoamine transporters based on this LC-ESI-MS/MS quantification method as read out. The affinities determined in saturation experiments for (R,R)-D-84 toward hDAT, for (S,S)-reboxetine toward hNET, and for (S)-citalopram toward hSERT, respectively, were in good accordance with results from literature, clearly demonstrating that the established MS Binding Assays have the potential to be an efficient alternative to radioligand binding assays widely used for this purpose so far.

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Hair testing in clinical setting: Simultaneous determination of 50 psychoactive drugs and metabolites in headache patients by LC tandem MS

Cited by 48 publications

References 37 publications

Segmental Hair Analysis—Interpretation of the Time of Drug Intake in Two Patients Undergoing Drug Treatment

Segmental Hair Analysis—Interpretation of the Time of Drug Intake in Two Patients Undergoing Drug Treatment

Monitoring of adherence to headache treatments by means of hair analysis

Development and validation of an LC‐ESI‐MS/MS method for the quantification of D‐84, reboxetine and citalopram for their use in MS Binding Assays addressing the monoamine transporters hDAT, hSERT and hNET

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