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Special Issue "Forensic Analysis in Chemistry"

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A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Medicinal Chemistry".

Deadline for manuscript submissions: 31 August 2023 | Viewed by 8476

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Special Issue Editors

Dr. Alexandre Quintas

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Centro de Investigação Interdisciplinar Egas Moniz (CiiEM), Egas Moniz, CRL, Monte de Caparica, Portugal
Interests: forensic toxicology; drugs of abuse; novel psychoactive substances; toxicological assays; forensic chemistry

Dr. Samir Ahmad

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Guest Editor

1. Centro de Investigação Interdisciplinar Egas Moniz (CiiEM), Egas Moniz, CRL, Monte de Caparica, Portugal
2. Centro de Química Estrutural, Institute of Molecular Sciences, Departamento de Química e Bioquímica, Faculdade de Ciências, Universidade de Lisboa, Lisboa, Portugal
Interests: forensic chemistry; chromatography; capillary electrophoresis; sample preparation; toxicology; drugs of abuse; contaminants; pollutants

Dr. Carla Ferreira

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Special Issue Information

Dear Colleagues,

Globalization has dramatically changed the crime landscape all around the world. Today, national, and transnational crime makes forensic investigations even more complex. This is especially true in forensic chemistry, where the appearance of new psychoactive substances on the market almost every week, the occurrence of unlawful discharges of multicompounds on the environment, food adulteration and contamination, the use of more complex explosives and precursors, and, at the same time, acknowledgement of the benefits as well as the restraints of laboratory certification and accreditation make the work of forensic analysts in chemistry even more challenging.

This Special Issue of Molecules welcomes original research articles, communications, and review articles dealing with research on the topics discussed above, as well as in all other fields in chemistry applied to solving forensic issues, including drug analysis, safe consumption, suspected documents, ink profiling and aging, accelerant analysis, explosives, latent fingerprint revelation, thanatochemistry, wastewater-based epidemiology, and forensic chemometrics. We are certain that this will be an excellent forum for providing and discussing recent developments in the field.

Dr. Alexandre Quintas
Dr. Samir Ahmad
Dr. Carla Ferreira
Guest Editors

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Keywords

new psychoactive substances
drugs of abuse
toxicology
pollution
explosives
inks
documents
fingerprinting
chemometrics
accreditation

Published Papers (9 papers)

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Research

Open AccessArticle

Determination of Phosphodiesterase Type-5 Inhibitors (PDE-5) in Dietary Supplements

Oana Ramona Cătălina Gheorghiu

Anne Marie Ciobanu

Claudia Maria Guțu

Carmen Lidia Chițescu

Giorgiana Valentina Costea

Daniela Mădălina Anghel

Ana Maria Vlasceanu

and

Daniela Luiza Baconi

Molecules 2023, 28(10), 4116; https://doi.org/10.3390/molecules28104116 - 16 May 2023

Viewed by 439

Abstract

This study proposed a high-performance thin-layer chromatography (HPTLC) screening method to detect phosphodiesterase 5 (PDE-5) inhibitors as possible adulterant agents in various dietary supplements. Chromatographic analysis was performed on silica gel 60F254 plates using a mixture of ethyl acetate:toluene:methanol:ammonia in a volume ratio of 50:30:20:0.5 as a mobile phase. The system provided compact spots and symmetrical peaks of sildenafil and tadalafil with retardation factor values of 0.55 and 0.90, respectively. The analysis of products purchased from the internet or specialized stores demonstrated the presence of sildenafil, tadalafil, or both compounds in 73.3% of products, highlighting inadequacies and inconsistencies in the labeling, as all dietary supplements were declared to be natural. The results were confirmed using ultra-high-performance liquid chromatography coupled with a positive electrospray ionization high-resolution tandem mass spectrometry (UHPLC-HRMS-MS) method. Furthermore, in some samples, vardenafil and various analogs of PDE-5 inhibitors were detected using a non-target HRMS-MS approach. The results of the quantitative analysis revealed similar findings between the two methods, with adulterant quantities found to be similar to or higher than those in approved medicinal products. This study demonstrated that the HPTLC method is a suitable and economical method for screening PDE-5 inhibitors as adulterants in dietary supplements intended for sexual activity enhancement. Full article

(This article belongs to the Special Issue Forensic Analysis in Chemistry)

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Open AccessArticle

Simple Method for the Determination of THC and THC-COOH in Human Postmortem Blood Samples by Gas Chromatography—Mass Spectrometry

Ivan Álvarez-Freire

Anxa Valeiras-Fernández

Pamela Cabarcos-Fernández

Ana María Bermejo-Barrera

and

María Jesús Tabernero-Duque

Molecules 2023, 28(8), 3586; https://doi.org/10.3390/molecules28083586 - 20 Apr 2023

Viewed by 429

Abstract

A simple and sensitive analytical method was developed for qualitative and quantitative analysis of Δ9-tetrahydrocannabinol (Δ9-THC) and its metabolite 11-nor-Δ9-tetrahydrocannabinol-carboxylic acid (Δ9-THC-COOH) in human postmortem blood using gas chromatography/mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. The method involved a liquid-liquid extraction in two steps, one for Δ9-THC and a second one for Δ9-THC-COOH. The first extract was analyzed using Δ9-THC-D3 as internal standard. The second extract was derivatized and analyzed using Δ9-THC-COOH-D3 as internal standard. The method was shown to be very simple, rapid, and sensitive. The method was validated for the two compounds, including linearity (range 0.05–1.5 µg/mL for Δ9-THC and 0.08–1.5 µg/mL for Δ9-THC-COOH), and the main precision parameters. It was linear for both analytes, with quadratic regression of calibration curves always higher than 0.99. The coefficients of variation were less than 15%. Extraction recoveries were superior to 80% for both compounds. The developed method was used to analyze 41 real plasma samples obtained from the Forensic Toxicology Service of the Institute of Forensic Sciences of Santiago de Compostela (Spain) from cases in which the use of cannabis was involved, demonstrating the usefulness of the proposed method. Full article

(This article belongs to the Special Issue Forensic Analysis in Chemistry)

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Open AccessArticle

New Trend in Toxicological Screening Using Volumetric Absorptive Microsampling (VAMS) and High-Resolution Mass Spectrometry (HR/MS) Combination

and

Molecules 2023, 28(8), 3466; https://doi.org/10.3390/molecules28083466 - 14 Apr 2023

Viewed by 529

Abstract

In toxicology, screenings are routinely performed using chromatographic methods coupled to detection systems such as high-resolution mass spectrometry (HR/MS). The increase in specificity and sensitivity of HRMS is responsible for the development of methods for alternative samples such as Volumetric Adsorptive Micro-Sampling. Whole blood overloaded with 90 drugs was sampled with 20 µL Mitra^TM to optimize the pre-analytical step as well as to determine the identification limits of drugs. Elution of chemicals was carried out in a solvent mixture through agitation and sonication. After dissolution, 10 μL was injected into the chromatographic system coupled to the Orbitrap^TM HR/MS. Compounds were confirmed against the laboratory library. The clinical feasibility was assessed in fifteen poisoned patients using the simultaneous sampling of plasma, whole blood and Mitra^TM. The optimized extraction procedure allowed us to confirm 87 compounds out of the 90 present in the spiked whole blood. Cannabis derivatives were not detected. For 82.2% of the investigated drugs, the identification limits were below 12.5 ng·mL⁻¹, with the extraction yields ranging from 80.6 to 108.7%. Regarding the patients’ analysis, 98% of the compounds in plasma were detected in Mitra^TM compared to whole blood, with a satisfying concordance (R² = 0.827). Our novel screening approach opens new insights into different toxicologic fields appropriate for pediatrics, forensics or to perform mass screening. Full article

(This article belongs to the Special Issue Forensic Analysis in Chemistry)

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Open AccessArticle

MALDI MSI Separation of Same Donor’s Fingermarks Based on Time of Deposition—A Proof-of-Concept Study

Kim Frisch

Kristine Lykke Nielsen

and

Simona Francese

Molecules 2023, 28(6), 2763; https://doi.org/10.3390/molecules28062763 - 19 Mar 2023

Viewed by 747

Abstract

Despite the advent of DNA profiling, fingerprints still play an important role in suspect identification. However, if single crime scene marks may be challenging to identify, overlapping fingermarks, understandably, pose an even greater challenge. In the last decade, mass spectrometry-imaging methods have provided a possible solution to the separation of fingermarks from two or more donors, based on the differential chemical composition. However, there are no studies attempting to separate overlapping marks from the same donor. This is important in relation to fingermark deposition at different times, which could be critical, for example, to ascertain legitimate access to the scene. In the work presented here, we investigate whether Matrix-Assisted Laser Desorption Ionisation Mass Spectrometry Imaging can separate the same donor’s fingermarks deposited at different times based on intra-donor fingermark composition variability. Additionally, the hypothesis that the different times of deposition could be also determined was investigated in the view of linking the suspect at the scene at different times; the dating window of MALDI MSI within the selected molecular range was explored. Results show that it is possible to separate overlapping fingermarks from the same donor in most cases, even from natural marks. Fresh marks (0 days) could be separated from those of fourteen days of age, though the latter could not be distinguished from the set aged for seven days. Due to the use of only one donor, these are to be considered preliminary data, though findings are interesting enough to warrant further investigation of the capabilities and limitations of this approach using a larger cohort of donors. Full article

(This article belongs to the Special Issue Forensic Analysis in Chemistry)

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Open AccessArticle

Analysis of Drugs in Saliva of US Military Veterans Treated for Substance Use Disorders Using Supported Liquid Extraction and Surface-Enhanced Raman Spectral Analysis

and

Molecules 2023, 28(5), 2010; https://doi.org/10.3390/molecules28052010 - 21 Feb 2023

Viewed by 803

Abstract

According to the Center for Disease Control, there were more than 107,000 US drug overdose deaths in 2021, over 80,000 of which due to opioids. One of the more vulnerable populations is US military veterans. Nearly 250,000 military veterans suffer from substance-related disorders (SRD). For those seeking treatment, buprenorphine is prescribed to help treat opioid use disorder (OUD). Urinalysis is currently used to monitor buprenorphine adherence as well as to detect illicit drug use during treatment. Sometimes sample tampering occurs if patients seek to generate a false positive buprenorphine urine test or mask illicit drugs, both of which can compromise treatment. To address this problem, we have been developing a point-of-care (POC) analyzer that can rapidly measure both medications used for treatment and illicit drugs in patient saliva, ideally in the physi-cian’s office. The two-step analyzer employs (1) supported liquid extraction (SLE) to isolate the drugs from the saliva and (2) surface-enhanced Raman spectroscopy (SERS) to detect the drugs. A prototype SLE-SERS-POC analyzer was used to quantify buprenorphine at ng/mL concentrations and identify illicit drugs in less than 1 mL of saliva collected from 20 SRD veterans in less than 20 min. It correctly detected buprenorphine in 19 of 20 samples (18 true positives, 1 true negative and 1 false negative). It also identified 10 other drugs in patient samples: acetaminophen, amphetamine, cannabidiol, cocaethylene, codeine, ibuprofen, methamphetamine, methadone, nicotine, and norbuprenorphine. The prototype analyzer shows evidence of accuracy in measuring treatment medications and relapse to drug use. Further study and development of the system is warranted. Full article

(This article belongs to the Special Issue Forensic Analysis in Chemistry)

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Open AccessArticle

GC-MS Analysis of Methadone and EDDP in Addicted Patients under Methadone Substitution Treatment: Comparison of Urine and Plasma as Biological Samples

Daniela-Mădălina Ciucă Anghel

and

Molecules 2022, 27(23), 8360; https://doi.org/10.3390/molecules27238360 - 30 Nov 2022

Cited by 1 | Viewed by 860

Abstract

(1) Background: Methadone, along with buprenorphine, is the most commonly used drug for the treatment of opioid dependence. This study aimed to analyze methadone and its major metabolite, 2-ethylidene-1,5-dimethyl-3,3-diphenyl pyrrolidine (EDDP), in the urine and plasma of opiate addicts. The study group consisted of drug users voluntarily admitted to the detoxification center C.E.T.T.T. “St. Stelian” of Bucharest. Secondly, the study aimed to identify whether urine or plasma provides better results for the proposed method. (2) Methods: A GC-MS method, using an internal standard (diphenylamine) in the FULL-SCAN and SIM modes of operation and using the m/z = 72 ion for methadone and the m/z = 277 ion for EDDP, combined with a liquid–liquid extraction procedure was performed. (3) Results: The applied procedure allows the detection and quantification of methadone in both urine and plasma samples. EDDP was identified in patients with higher levels of methadone. Higher levels of methadone were detected in urine than in plasma samples. (4) Conclusions: This procedure can be used in clinical laboratories for the rapid determination of methadone levels in urine rather than in plasma. The procedure can be applied for the monitoring of methadone substitution treatment. Full article

(This article belongs to the Special Issue Forensic Analysis in Chemistry)

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Open AccessArticle

Determination of Mifepristone (RU-486) and Its Metabolites in Maternal Blood Sample after Pharmacological Abortion

and

Molecules 2022, 27(21), 7605; https://doi.org/10.3390/molecules27217605 - 06 Nov 2022

Viewed by 1426

Abstract

The aim of the study was the development and validation of the UHPLC-QqQ-MS/MS method for the determination of mifepristone in human blood as well as the identification and quantification of its metabolites after self-induced pharmacological abortion. The metabolic pathway in humans was proposed after examination of an authentic casework. The fast and simple preanalytical procedure was successfully applied (pH9, tert-butyl-methyl ether). The validation parameters of the method were as follows: limit of quantification: 0.5 ng/mL; coefficients of determination: >0.999 (R²), intra- and inter-day accuracy and precision values did not exceed ± 13.2%. The recovery and matrix effect were in the range of 96.3–114.7% and from −3.0 to 14.7%, respectively. Toxicological analysis of the mother’s blood (collected the day after the pregnancy termination) revealed the presence of five compounds: mifepristone (557.4 ng/mL), N-desmethyl-mifepristone (638.7 ng/mL), 22-OH-mifepristone (176.9 ng/mL), N,N-didesmethyl-mifepristone (144.5 ng/mL) and N-desmethyl-hydroxy-mifepristone (qualitatively). To our knowledge, the study presented in this paper is the first report on the concentrations of mifepristone and its metabolites in maternal blood samples after performing a self-induced abortion. The established UHPLC-QqQ-MS/MS method is suitable for forensic toxicological analysis as well as in terms of clinical toxicology in future investigations (examination of pharmacokinetics, bioavailability and metabolism of RU-486). Full article

(This article belongs to the Special Issue Forensic Analysis in Chemistry)

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Open AccessArticle

Rapid Determination of Non-Steroidal Anti-Inflammatory Drugs in Urine Samples after In-Matrix Derivatization and Fabric Phase Sorptive Extraction-Gas Chromatography-Mass Spectrometry Analysis

and

Molecules 2022, 27(21), 7188; https://doi.org/10.3390/molecules27217188 - 24 Oct 2022

Cited by 5 | Viewed by 1003

Abstract

Fabric phase sorptive extraction (FPSE) has become a popular sorptive-based microextraction technique for the rapid analysis of a wide variety of analytes in complex matrices. The present study describes a simple and green analytical protocol based on in-matrix methyl chloroformate (MCF) derivatization of non-steroidal anti-inflammatory (NSAID) drugs in urine samples followed by FPSE and gas chromatography-mass spectrometry (GC-MS) analysis. Use of MCF as derivatizing reagent saves substantial amounts of time, reagent and energy, and can be directly performed in aqueous samples without any sample pre-treatment. The derivatized analytes were extracted using sol–gel Carbowax 20M coated FPSE membrane and eluted in 0.5 mL of MeOH for GC-MS analysis. A chemometric design of experiment-based approach was utilized comprising a Placket–Burman design (PBD) and central composite design (CCD) for screening and optimization of significant variables of derivatization and FPSE protocol, respectively. Under optimized conditions, the proposed FPSE-GC-MS method exhibited good linearity in the range of 0.1–10 µg mL⁻¹ with coefficients of determination (R²) in the range of 0.998–0.999. The intra-day and inter-day precisions for the proposed method were lower than <7% and <10%, respectively. The developed method has been successfully applied to the determination of NSAIDs in urine samples of patients under their medication. Finally, the green character of the proposed method was evaluated using ComplexGAPI tool. The proposed method will pave the way for simper analysis of polar drugs by FPSE-GC-MS. Full article

(This article belongs to the Special Issue Forensic Analysis in Chemistry)

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Open AccessArticle

Forensic Toxicological Aspects of Misoprostol Use in Pharmacological Abortions

Paweł Szpot

Olga Wachełko

and

Marcin Zawadzki

Molecules 2022, 27(19), 6534; https://doi.org/10.3390/molecules27196534 - 03 Oct 2022

Cited by 1 | Viewed by 1494

Abstract

The aim of this study was establishment of an UHPLC-QqQ-MS/MS method for the deter-mination of misoprostol acid in biological specimens in cases of pharmacological abortions. Forensic toxicological examination was performed in three different biological samples (whole blood, placenta and fetal liver). The validation parameters of the method were as follows: limit of detection: 25 pg/mL; limit of quantification: 50 pg/mL, coefficient of determination: >0.999 (R²), intra- and interday accuracy and precision: not greater than 13.7%. The recovery and matrix effect were in the range of 88.3–95.1% and from −11.7 to −4.9%, respectively. Toxicological analysis of the mother’s blood (collected two days after pregnancy termination) did not reveal any abortifacients; however, misoprostol acid was found in the placenta (793 pg/g) and fetal liver (309 pg/g). The second case involved a fetus found near a garbage container. The concentration of misoprostol acid in the placenta was 2332 pg/g. In the presented study, an extensive literature review of misoprostol pharmacokinetics studies was performed. To our knowledge, the UHPLC-QqQ-MS/MS technique presented in this paper is the first quantitative method applied for forensic toxicological purposes. In addition, postmortem concentrations of misoprostol acid in miscarried fetuses due to illegal abortions were reported for the first time. Full article

(This article belongs to the Special Issue Forensic Analysis in Chemistry)

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