Simultaneous Quantification of 25 Fentanyl Derivatives and Metabolites in Oral Fluid by Means of Microextraction on Packed Sorbent and LC–HRMS/MS Analysis

Fentanyl and fentalogs’ intake as drugs of abuse is experiencing a great increase in recent years. For this reason, there are more and more cases in which it is important to recognize and quantify these molecules and related metabolites in biological matrices. Oral fluid (OF) is often used to find out if a subject has recently used a psychoactive substance and if, therefore, the person is still under the effect of psychotropics. Given its difficulty in handling, good sample preparation and the development of instrumental methods for analysis are essential. In this work, an analytical method is proposed for the simultaneous determination of 25 analytes, including fentanyl, several derivatives and metabolites. OF was collected by means of passive drool; sample pretreatment was developed in order to be fast, simple and possibly semi-automated by exploiting microextraction on packed sorbent (MEPS). The analysis was performed by means of LC–HRMS/MS obtaining good identification and quantification of all the analytes in less than 10 min. The proposed method was fully validated according to the Scientific Working Group for Forensic Toxicology (SWGTOX) international guidelines. Good results were obtained in terms of recoveries, matrix effect and sensitivity, showing that this method could represent a useful tool in forensic toxicology. The presented method was successfully applied to the analysis of proficiency test samples.

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Simultaneous and Sensitive Determination of Amphetamine, Codeine and Morphine in Exhaled Breath Condensate, Using Capillary Electrophoresis Coupled with On-line and Off-line Enhancing Methods

Current Pharmaceutical Analysis ◽

10.2174/1573412915666190219143049 ◽

2020 ◽

Vol 16 (7) ◽

pp. 872-879

Author(s):

Samin Hamidi

Keyword(s):

Drugs Of Abuse ◽

Exhaled Breath Condensate ◽

Direct Injection ◽

Forensic Toxicology ◽

Analytical Signal ◽

Exhaled Breath ◽

Concentration Method ◽

Validation Parameters ◽

Breath Condensate

Background: Abuse of drugs is associated with several medical, forensic, toxicology and social challenges. “Drugs of abuse” testing is therefore an important issue. Objective: We propose a simple CE-based method for the quantification of amphetamine, codeine and morphine after direct injection of Exhaled Breath Condensate (EBC) by the aid of simple stacking mode and an off-line pre-concentration method. Methods: Using graphene oxide adsorbents, amphetamine, codeine and morphine were extracted from EBC in order to eliminate the proteins and other interferences. In addition to off-line method, an online stacking mode was applied to improve the analytical signal obtained from the instrument. Results: The validation parameters were experimented on the developed method based on the FDA guideline over concentration ranges of 12.5-100, 30-500 and 10-1250 ng/mL associated with amphetamine, codeine and morphine, respectively. Small volumes (around 100 μL) of EBC were collected using a lab-made setup and successfully analyzed using the proposed method where precisions and accuracies (within day and between days) were in accordance with the guideline (recommended less than 15 % for biological samples). The recovery tests were used to evaluate the matrix effect and data (94 to 105 %) showed that the proposed method can be applied in different EBC matrix samplings of subjects. Conclusion: The proposed method is superior for simultaneous determination of amphetamine, codeine and morphine over chromatographic analyses because it is fast and consumes fewer chemicals, with no derivatization step.

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A new LC-MS/MS confirmation method for the determination of 17 drugs of abuse in oral fluid and its application to real samples

Forensic Science International ◽

10.1016/j.forsciint.2020.110330 ◽

2020 ◽

Vol 312 ◽

pp. 110330

Author(s):

Elisa Bassotti ◽

Giuseppe Maria Merone ◽

Annachiara D’Urso ◽

Fabio Savini ◽

Marcello Locatelli ◽

...

Keyword(s):

Oral Fluid ◽

Drugs Of Abuse ◽

Real Samples

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Validated toxicological determination of 30 drugs of abuse as optimized derivatives in oral fluid by long column fast gas chromatography/electron impact mass spectrometry

Journal of Mass Spectrometry ◽

10.1002/jms.846 ◽

2005 ◽

Vol 40 (6) ◽

pp. 739-753 ◽

Cited By ~ 89

Author(s):

Teemu Gunnar ◽

Kari Ariniemi ◽

Pirjo Lillsunde

Keyword(s):

Mass Spectrometry ◽

Gas Chromatography ◽

Electron Impact ◽

Oral Fluid ◽

Drugs Of Abuse ◽

Electron Impact Mass Spectrometry ◽

Fast Gas Chromatography ◽

Electron Impact Mass ◽

Impact Mass

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Determination of the Synthetic Cannabinoids JWH-122, JWH-210, UR-144 in Oral Fluid of Consumers by GC-MS and Quantification of Parent Compounds and Metabolites by UHPLC-MS/MS

International Journal of Molecular Sciences ◽

10.3390/ijms21249414 ◽

2020 ◽

Vol 21 (24) ◽

pp. 9414

Author(s):

Nunzia La Maida ◽

Manuela Pellegrini ◽

Esther Papaseit ◽

Clara Pérez-Mañá ◽

Lourdes Poyatos ◽

...

Keyword(s):

Mass Spectrometry ◽

High Performance ◽

Oral Fluid ◽

High Resolution Mass Spectrometry ◽

Synthetic Cannabinoids ◽

Screening Method ◽

Forensic Toxicology ◽

Gas Chromatography Mass Spectrometry ◽

Limit Of Quantification

The consumption of synthetic cannabinoids (SCs) has significantly increased in the last decade and the analysis of SCs and their metabolites in human specimens is gaining interest in clinical and forensic toxicology. A pilot study has been carried out using a combination of an initial last generation gas chromatography-mass spectrometry (GC-MS) screening method for the determination of JWH-122, JWH-210, UR-144) in oral fluid (OF) of consumers and an ultra-high performance liquid chromatography high resolution mass spectrometry (UHPLC-HRMS) confirmatory method for the quantification of the parent compounds and their metabolites in the same biological matrix. OF samples were simply liquid-liquid extracted before injecting in both chromatographic systems. The developed methods have been successfully validated and were linear from limit of quantification (LOQ) to 50 ng/mL OF. Recovery of analytes was always higher than 70% and matrix effect always lower than 15% whereas intra-assay and inter-assay precision and accuracy were always better than 16%. After smoking 1 mg JWH-122 or UR-144 and 3 mg JWH-210, maximum concentration of 4.00–3.14 ng/mL JWH-122, 8.10–7.30 ng/mL JWH-210 ng/mL and 7.40 and 6.81 ng/mL UR-144 were measured by GC-MS and UHPLC-HRMS respectively at 20 min after inhalation. Metabolites of JWH 122 and 210 were quantified in OF by UHPLC-HRMS, while that of UR144 was only detectable in traces. Our results provide for the first time information about disposition of these SCs and their metabolites in consumers OF. Last generation GC-MS has proven useful tool to identify and quantify parent SCs whereas UHPLC-HRMS also confirmed the presence of SCs metabolites in the OF of SCs consumers.

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A comparison between two different dried blood substrates in determination of psychoactive substances in postmortem samples

Forensic Toxicology ◽

10.1007/s11419-020-00567-2 ◽

2021 ◽

Author(s):

Matteo Moretti ◽

Alessandro Manfredi ◽

Francesca Freni ◽

Carlo Previderé ◽

Antonio Marco Maria Osculati ◽

...

Keyword(s):

Drugs Of Abuse ◽

Forensic Toxicology ◽

Dried Blood Spots ◽

Psychoactive Substances ◽

Extraction Solvent ◽

Quantitative Correlation ◽

Fta Cards ◽

Postmortem Blood ◽

Quantitative Results

Abstract Purpose Whatman™ 903 cards represent a valid type of support for collection, storage, and analysis of dried blood spots (DBS). Whatman™ FTA (Flinders Technology Associates) are a type of cards soaked in chemicals that cause denaturation of proteins, while preserving DNA and ensuring the safe handling of DBS; to date, these cards are still rarely employed in forensic toxicology. The aim of this study was to analyze several psychoactive substances on not-dried blood on the two different cards and to compare the qualitative and quantitative results. Methods Twenty cardiac postmortem blood samples were collected and deposed on Whatman™ 903 and Whatman™ FTA cards. Spots and not-dried blood were analyzed following our validated and previously published liquid chromatography–mass spectrometry methods. Results We were able to identify: eight drugs of abuse and their metabolites (15 cases), five benzodiazepines and their metabolites (3 cases), six antidepressants (6 cases) and two antipsychotics (3 cases). We observed a perfect qualitative correspondence and a general good quantitative correlation between data obtained from not-dried blood and the two different DBS cards, except for alprazolam, diazepam, desmethyldiazepam, fluoxetine and sertraline, that showed a lower concentration on FTA. Additional experiments suggest that the chemicals, adsorbed on FTA, are not the cause of the loss of signal observed for the substances previously mentioned and that methanol should be preferred as extraction solvent. Conclusions This study proved that FTA cards are a good and a hazard-free alternative sample storage method for analysis of several psychoactive substances in postmortem blood.

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Determination of Third-Generation Synthetic Cannabinoids in Oral Fluids

Journal of Analytical Toxicology ◽

10.1093/jat/bkaa091 ◽

2020 ◽

Cited By ~ 3

Author(s):

Aitor Sorribes-Soriano ◽

Josep Verdeguer ◽

Agustín Pastor ◽

Sergio Armenta ◽

Francesc A Esteve-Turrillas

Keyword(s):

Oral Fluid ◽

Synthetic Cannabinoids ◽

High Sensitivity ◽

Gas Chromatography Mass Spectrometry ◽

Third Generation ◽

Model Compounds ◽

Oral Fluids ◽

Sensitive Determination ◽

Packed Sorbent

Abstract A procedure has been developed for the determination of third-generation synthetic cannabinoids in oral fluid samples by using a semi-automated microextraction by packed sorbent (MEPS) procedure and gas chromatography–mass spectrometry (GC–MS) determination. Five synthetic cannabinoids were employed as model compounds 5F-ADB, MMB-CHMICA, THJ-2201, CUMYL-4CN-BINACA and MDMB-CHMCZCA. The most adequate operative conditions for MEPS were evaluated giving quantitative recoveries, from 89 to 124%, in synthetic and field saliva samples spiked with 125 and 250 μg/L of the studied cannabinoids, with the exception of MDMB-CHMCZCA in field saliva samples that provided slightly lower recoveries from 62 to 66%. A high sensitivity was obtained for the proposed MEPS-GC–MS procedure with limits of detection from 10 to 20 μg/L. The obtained results demonstrate the high potential of MEPS-GC–MS combination for semi-automated, selective and sensitive determination of synthetic cannabinoids in oral fluid samples.

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Alternative matrices in forensic toxicology: a critical review

Forensic Toxicology ◽

10.1007/s11419-021-00596-5 ◽

2021 ◽

Author(s):

Eduardo Geraldo de Campos ◽

Bruno Ruiz Brandão da Costa ◽

Fabiana Spineti dos Santos ◽

Fernanda Monedeiro ◽

Marcela Nogueira Rabelo Alves ◽

...

Keyword(s):

Breast Milk ◽

Critical Review ◽

Oral Fluid ◽

Drug Exposure ◽

Drugs Of Abuse ◽

Recent Literature ◽

Forensic Toxicology ◽

Vitreous Humor ◽

Biological Matrices ◽

Alternative Matrices

Abstract Purpose The use of alternative matrices in toxicological analyses has been on the rise in clinical and forensic settings. Specimens alternative to blood and urine are useful in providing additional information regarding drug exposure and analytical benefits. The goal of this paper is to present a critical review on the most recent literature regarding the application of six common alternative matrices, i.e., oral fluid, hair, sweat, meconium, breast milk and vitreous humor in forensic toxicology. Methods The recent literature have been searched and reviewed for the characteristics, advantages and limitations of oral fluid, hair, sweat, meconium, breast milk and vitreous humor and its applications in the analysis of traditional drugs of abuse and novel psychoactive substances (NPS). Results This paper outlines the properties of six biological matrices that have been used in forensic analyses, as alternatives to whole blood and urine specimens. Each of this matrix has benefits in regards to sampling, extraction, detection window, typical drug levels and other aspects. However, theses matrices have also limitations such as limited incorporation of drugs (according to physical–chemical properties), impossibility to correlate the concentrations for effects, low levels of xenobiotics and ultimately the need for more sensitive analysis. For more traditional drugs of abuse (e.g., cocaine and amphetamines), there are already data available on the detection in alternative matrices. However, data on the determination of emerging drugs such as the NPS in alternative biological matrices are more limited. Conclusions Alternative biological fluids are important specimens in forensic toxicology. These matrices have been increasingly reported over the years, and this dynamic will probably continue in the future, especially considering their inherent advantages and the possibility to be used when blood or urine are unavailable. However, one should be aware that these matrices have limitations and particular properties, and the findings obtained from the analysis of these specimens may vary according to the type of matrix. As a potential perspective in forensic toxicology, the topic of alternative matrices will be continuously explored, especially emphasizing NPS.

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