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Advances on Bioanalysis: Recent Approaches in the Determination of Biomarkers, Drugs of Abuse and Medicines —Second Edition

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

Deadline for manuscript submissions: closed (31 August 2023) | Viewed by 16646

Special Issue Editors


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Guest Editor
Laboratory of Forensic Chemistry and Toxicology, National Institute of Legal Medicine and Forensic Sciences, I.P. – South Branch, Rua Manuel Bento de Sousa, n.º 3, 1169-201 Lisboa, Portugal
Interests: method development and validation; hair testing; alternative specimens; drug monitoring; toxicology
Special Issues, Collections and Topics in MDPI journals

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Guest Editor
1. Health Sciences Research Centre, University of Beira Interior (CICS-UBI), Covilhã, Portugal
2. Pharmaco-Toxicology Laboratory, UBIMedical, University of Beira Interior, Covilhã, Portugal
3. Centro Académico Clínico das Beiras (CACB)—Grupo de Problemas Relacionados com Toxicofilias, Covilhã, Portugal
Interests: toxicology; analytical method development; recreational drugs; natural psychoactive substances; therapeutic drug monitoring; sample preparation; alternative samples; miniaturized extraction procedures
Special Issues, Collections and Topics in MDPI journals

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Guest Editor
1. Associate Laboratory i4HB—Institute for Health and Bioeconomy, NOVA School of Science and Technology, Universidade NOVA de Lisboa, 2819-516 Caparica, Portugal
2. UCIBIO—Applied Molecular Biosciences Unit, Chemistry Department, NOVA School of Science and Technology, Universidade NOVA de Lisboa, 2829-516 Caparica, Portugal
3. CICS-UBI—Health Sciences Research Centre, University of Beira Interior, 6201-506 Covilhã, Portugal
Interests: method development and validation; electrochemical detection; proteomics; protein biomarkers
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Analytical tools to determine drugs, drugs of abuse, or biomarkers for the rapid diagnosis of intoxications or diseases are mandatory for every laboratory working in the bioanalytical field. In the last few years, the development of sensible analytical instrumentation (e.g., time of flight, high-resolution mass spectrometry, or Orbitrap mass spectrometers) has widened the scope of applications of such techniques to several areas, for instance, in the development of new therapeutic agents, industry, and others. This progress concerning instrumentation was also accompanied by important achievements related to sample preparation approaches, namely, trending in low-sample, low-cost, and low-organic solvent procedures without compromising sensitivity and allowing the analysis of alternative samples, such as exhaled breath, hair, oral fluid, or sweat. Due to the great success of the first edition of the Special Issue on “Advances on Bioanalysis: Recent Approaches in the Determination of Biomarkers, Drugs of Abuse and Medicines”, it is our pleasure to announce this second edition.

Presenting a very broad scope, this Special Issue welcomes full papers, short communications, and review articles on, but not limited to, new developments in bioanalysis, sample preparation, and the development of new detection and quantification of disease biomarkers, toxic agents, and drug monitoring approaches with applications in different analytical fields.

This issue will be an excellent collection of papers for academia, or as a reference tool for researchers, particularly those working in the fields of medicine, biotechnology, pharmaceutical sciences, chemistry, and toxicology, including health and industry professionals.

We are looking forward to receiving your contributions.

Dr. Mário Barroso
Prof. Dr. Eugenia Gallardo
Dr. Luís Passarinha
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Molecules is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • bioanalysis
  • development of analytical methods
  • sample preparation techniques
  • biomarkers
  • toxics
  • drugs of abuse
  • drug monitoring

Published Papers (8 papers)

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Research

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12 pages, 2536 KiB  
Article
The Finding of New In Vivo Metabolite Triptorelin (5-10) in Human Urine Using Liquid Chromatography Coupled with Ion Trap/Time-of-Flight Mass Spectrometry with Dimethyl Sulfoxide Additives in the Mobile Phase
by Navaporn Saardpun, Ruamsiri Songsaeng, Pansakorn Tanratana, Thanit Kusamran and Darawan Pinthong
Molecules 2023, 28(12), 4572; https://doi.org/10.3390/molecules28124572 - 6 Jun 2023
Cited by 2 | Viewed by 1481
Abstract
Triptorelin and leuprorelin are synthetic gonadotrophin-releasing hormones (GnRH) that are on the World Anti-Doping Agency (WADA) list of prohibited substances. To investigate the possible in vivo metabolites of triptorelin and leuprorelin in humans compared to previously reported in vitro metabolites, excreted urine from [...] Read more.
Triptorelin and leuprorelin are synthetic gonadotrophin-releasing hormones (GnRH) that are on the World Anti-Doping Agency (WADA) list of prohibited substances. To investigate the possible in vivo metabolites of triptorelin and leuprorelin in humans compared to previously reported in vitro metabolites, excreted urine from five patients treated with either triptorelin or leuprorelin was analyzed by liquid chromatography coupled with ion trap/time-of-flight mass spectrometry (LC/MS-IT-TOF). The addition of dimethyl sulfoxide (DMSO) to the mobile phase was found to enhance the detection sensitivity of certain GnRH analogs. The method was validated, and the limit of detection (LOD) was found at 0.02−0.08 ng/mL. Using this method, a novel new metabolite of triptorelin was discovered in the urine of all subjects up to 1 month after triptorelin administration, but it was not observed in the urine of subjects before drug administration. The limit of detection was estimated to be 0.05 ng/mL. The structure of the metabolite, triptorelin (5-10), is proposed from bottom-up mass spectrometry analysis. The discovery of in vivo triptorelin (5-10) can possibly be used as supporting evidence of triptorelin misuse in athletes. Full article
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17 pages, 1989 KiB  
Article
Evaluation of Antipsychotic Drugs’ Stability in Oral Fluid Samples
by Carina Gameiro, Joana Gonçalves, Sofia Soares, Tiago Rosado, André R. T. S. Araujo, Luís A. Passarinha, Mário Barroso and Eugenia Gallardo
Molecules 2023, 28(5), 2030; https://doi.org/10.3390/molecules28052030 - 21 Feb 2023
Cited by 1 | Viewed by 1465
Abstract
Antipsychotics have narrow therapeutic windows, and their monitoring in biological fluids is therefore important; consequently, stability in those fluids must be investigated during method development and validation. This work evaluates the stability of chlorpromazine, levomepromazine, cyamemazine, clozapine, haloperidol, and quetiapine in oral fluid [...] Read more.
Antipsychotics have narrow therapeutic windows, and their monitoring in biological fluids is therefore important; consequently, stability in those fluids must be investigated during method development and validation. This work evaluates the stability of chlorpromazine, levomepromazine, cyamemazine, clozapine, haloperidol, and quetiapine in oral fluid (OF) samples, using the dried saliva spots (DSS) sampling approach and gas chromatography coupled to tandem mass spectrometry. Since many parameters can influence the stability of the target analytes, design of experiments was adopted to check the crucial factors that affect that stability in a multivariate fashion. The studied parameters were the presence of preservatives at different concentrations, temperature, light, and time. It was possible to observe that antipsychotic stability improved when OF samples in DSS were stored at 4 °C, with a low ascorbic acid concentration, and in the absence of light. With these conditions, chlorpromazine and quetiapine were stable for 14 days, clozapine and haloperidol were stable for 28 days, levomepromazine remained stable for 44 days, and cyamemazine was stable for the entire monitored period (146 days). This is the first study that evaluates the stability of these antipsychotics in OF samples after application to DSS cards. Full article
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17 pages, 645 KiB  
Article
Proteomics Analysis of Lymphoblastoid Cell Lines from Patients with Amyotrophic Lateral Sclerosis
by Danielle Whitham, Eugene Belenkiy, Costel C. Darie and Aurelian Radu
Molecules 2023, 28(5), 2014; https://doi.org/10.3390/molecules28052014 - 21 Feb 2023
Viewed by 1647
Abstract
Amyotrophic lateral sclerosis (ALS) consists of the progressive degeneration of motor neurons, caused by poorly understood mechanisms for which there is no cure. Some of the cellular perturbations associated with ALS can be detected in peripheral cells, including lymphocytes from blood. A related [...] Read more.
Amyotrophic lateral sclerosis (ALS) consists of the progressive degeneration of motor neurons, caused by poorly understood mechanisms for which there is no cure. Some of the cellular perturbations associated with ALS can be detected in peripheral cells, including lymphocytes from blood. A related cell system that is very suitable for research consists of human lymphoblastoid cell lines (LCLs), which are immortalized lymphocytes. LCLs that can be easily expanded in culture and can be maintained for long periods as stable cultures. We investigated, on a small set of LCLs, if a proteomics analysis using liquid chromatography followed by tandem mass spectrometry reveals proteins that are differentially present in ALS versus healthy controls. We found that individual proteins, the cellular and molecular pathways in which these proteins participate, are detected as differentially present in the ALS samples. Some of these proteins and pathways are already known to be perturbed in ALS, while others are new and present interest for further investigations. These observations suggest that a more detailed proteomics analysis of LCLs, using a larger number of samples, represents a promising approach for investigating ALS mechanisms and to search for therapeutic agents. Proteomics data are available via ProteomeXchange with identifier PXD040240. Full article
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16 pages, 3446 KiB  
Article
Application of Ionic Liquids as Mobile Phase Additives for Simultaneous Analysis of Nicotine and Its Metabolite Cotinine in Human Plasma by HPLC–DAD
by Roxana E. Axente, Miriana Stan, Carmen L. Chitescu, Viorela G. Nitescu, Ana-Maria Vlasceanu and Daniela L. Baconi
Molecules 2023, 28(4), 1563; https://doi.org/10.3390/molecules28041563 - 6 Feb 2023
Cited by 2 | Viewed by 1331
Abstract
Nicotine and cotinine are very polar basic molecules, which makes it difficult to analyze them by reversed-phase liquid chromatography (RPLC), especially in biological samples. Additives with an ionic character have been traditionally used in RPLC as silanol suppressors. The aim of our study [...] Read more.
Nicotine and cotinine are very polar basic molecules, which makes it difficult to analyze them by reversed-phase liquid chromatography (RPLC), especially in biological samples. Additives with an ionic character have been traditionally used in RPLC as silanol suppressors. The aim of our study was to investigate the potential of selected ionic liquids in improving chromatographic performance in comparison with common additives. The experimental design was conducted using the following ionic liquids as the mobile phase modifiers: 1-butyl-3-methylimidazolium tetrafluoroborate, BMIM[BF4] and 1-butyl-3-methylimidazolium hexafluorophosphate BMIM[PF6], with a C18 chromatographic column. The separation of these alkaloids on silica-based RPLC stationary phases was successfully conducted by the addition of BMIM[BF4] in an acetonitrile:phosphate-buffer-based mobile phase in a pH range of 2.3–5.2. The presented chromatographic method can be used as alternative for monitoring studies or pharmacokinetic application necessary for the evaluation of tobacco smoke exposure. Full article
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15 pages, 3792 KiB  
Article
Highly Sensitive ZnO/Au Nanosquare Arrays Electrode for Glucose Biosensing by Electrochemical and Optical Detection
by Vinda Zakiyatuz Zulfa, Nasori Nasori, Ulya Farahdina, Miftakhul Firdhaus, Ihwanul Aziz, Hari Suprihatin, Muslikha Nourma Rhomadhoni and Agus Rubiyanto
Molecules 2023, 28(2), 617; https://doi.org/10.3390/molecules28020617 - 7 Jan 2023
Cited by 5 | Viewed by 2285
Abstract
The fabrication of a ZnO/Au nanosquare-array electrode was successfully carried out for the detection of glucose concentration in biomedical applications. The fabrication of the ZnO/Au nanosquare array using an ultra-thin alumina mask (UTAM) based on the imprinted anodic aluminum oxide (AAO) template and [...] Read more.
The fabrication of a ZnO/Au nanosquare-array electrode was successfully carried out for the detection of glucose concentration in biomedical applications. The fabrication of the ZnO/Au nanosquare array using an ultra-thin alumina mask (UTAM) based on the imprinted anodic aluminum oxide (AAO) template and the direct current (DC) sputtering method was able to produce a very well-ordered nanosquare arrangement with a side size of 300 nm and a thickness of 100 nm. Tests were done to evaluate the performance of the electrode by means of cyclic voltammetry (CV) which showed that the addition of glucose oxidase (GOx) increased the sensitivity of the electrode up to 1180 ± 116 μA mM−1cm−2, compared with its sensitivity prior to the addition of GOx of 188.34 ± 18.70 mA mM−1 cm−2. A iox/ired ratio equal to ~1 between the peaks of redox reactions was obtained for high (hyperglycemia), normal, and low (hypoglycemia) levels of glucose. The ZnO/Au nanosquare-array electrode was 7.54% more sensitive than the ZnO/Au thin-film electrode. Furthermore, finite-difference time-domain (FDTD) simulations and theoretical calculations of the energy density of the electric and magnetic fields produced by the ZnO/Au electrode were carried out and compared to the results of CV. From the results of CV, FDTD simulation, and theoretical calculations, it was confirmed that the ZnO/Au nanosquare array possessed a significant optical absorption and that the quantum effect from the nanosquare array resulted in a higher sensitivity than the thin film. Full article
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18 pages, 7757 KiB  
Article
A Non-Instrumental Green Analytical Method Based on Surfactant-Assisted Dispersive Liquid–Liquid Microextraction–Thin-Layer Chromatography–Smartphone-Based Digital Image Colorimetry(SA-DLLME-TLC-SDIC) for Determining Favipiravir in Biological Samples
by Bharti Jain, Rajeev Jain, Prashant Kumar Jaiswal, Torki Zughaibi, Tanvi Sharma, Abuzar Kabir, Ritu Singh and Shweta Sharma
Molecules 2023, 28(2), 529; https://doi.org/10.3390/molecules28020529 - 5 Jan 2023
Cited by 13 | Viewed by 2778
Abstract
Favipiravir (FAV) has become a promising antiviral agent for the treatment of COVID-19. Herein, a green, fast, high-sample-throughput, non-instrumental, and affordable analytical method is proposed based on surfactant-assisted dispersive liquid–liquid microextraction (SA-DLLME) combined with thin-layer chromatography–digital image colourimetry (TLC-DIC) for determining favipiravir in [...] Read more.
Favipiravir (FAV) has become a promising antiviral agent for the treatment of COVID-19. Herein, a green, fast, high-sample-throughput, non-instrumental, and affordable analytical method is proposed based on surfactant-assisted dispersive liquid–liquid microextraction (SA-DLLME) combined with thin-layer chromatography–digital image colourimetry (TLC-DIC) for determining favipiravir in biological and pharmaceutical samples. Triton X-100 and dichloromethane (DCM) were used as the disperser and extraction solvents, respectively. The extract obtained after DLLME procedure was spotted on a TLC plate and allowed to develop with a mobile phase of chloroform:methanol (8:2, v/v). The developed plate was photographed using a smartphone under UV irradiation at 254 nm. The quantification of FAV was performed by analysing the digital images’ spots with open-source ImageJ software. Multivariate optimisation using Plackett–Burman design (PBD) and central composite design (CCD) was performed for the screening and optimisation of significant factors. Under the optimised conditions, the method was found to be linear, ranging from 5 to 100 µg/spot, with a correlation coefficient (R2) ranging from 0.991 to 0.994. The limit of detection (LOD) and limit of quantification (LOQ) were in the ranges of 1.2–1.5 µg/spot and 3.96–4.29 µg/spot, respectively. The developed approach was successfully applied for the determination of FAV in biological (i.e., human urine and plasma) and pharmaceutical samples. The results obtained using the proposed methodology were compared to those obtained using HPLC-UV analysis and found to be in close agreement with one another. Additionally, the green character of the developed method with previously reported protocols was evaluated using the ComplexGAPI, AGREE, and Eco-Scale greenness assessment tools. The proposed method is green in nature and does not require any sophisticated high-end analytical instruments, and it can therefore be routinely applied for the analysis of FAV in various resource-limited laboratories during the COVID-19 pandemic. Full article
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14 pages, 631 KiB  
Article
Antitrypanosomal, Antitopoisomerase-I, and Cytotoxic Biological Evaluation of Some African Plants Belonging to Crassulaceae; Chemical Profiling of Extract Using UHPLC/QTOF-MS/MS
by Mostafa M. Hegazy, Wael M. Afifi, Ahmed M. Metwaly, Mohamed M. Radwan, Muhamad Abd-Elraouf, Ahmed B. M. Mehany, Eman Ahmed, Shymaa Enany, Shahd Ezzeldin, Adel E. Ibrahim, Sami El Deeb and Ahmad E. Mostafa
Molecules 2022, 27(24), 8809; https://doi.org/10.3390/molecules27248809 - 12 Dec 2022
Cited by 5 | Viewed by 2104
Abstract
In our continuous study for some African plants as a source for antitrypanosomally and cytotoxic active drugs, nine different plants belonging to the Crassulaceae family have been selected for the present study. Sedum sieboldii leaves extract showed an antitrypanosomal activity against Trypanosoma brucei [...] Read more.
In our continuous study for some African plants as a source for antitrypanosomally and cytotoxic active drugs, nine different plants belonging to the Crassulaceae family have been selected for the present study. Sedum sieboldii leaves extract showed an antitrypanosomal activity against Trypanosoma brucei with an IC50 value of 8.5 µg/mL. In addition, they have cytotoxic activities against (HCT-116), (HEPG-2) and (MCF-7), with IC50 values of 28.18 ± 0.24, 22.05 ± 0.66, and 26.47 ± 0.85 µg/mL, respectively. Furthermore, the extract displayed inhibition against Topoisomerase-1 with an IC50 value of 1.31 µg/mL. It showed the highest phenolics and flavonoids content among the other plants’ extracts. In order to identify the secondary metabolites which may be responsible for such activities, profiling of the polar secondary metabolites of S. sieboldii extract via Ultra-Performance Liquid Chromatography coupled to High-Resolution QTOF-MS operated in negative and positive ionization modes, which revealed the presence of 46 metabolites, including flavonoids, phenolic acids, anthocyanidins, coumarin, and other metabolites. Full article
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Review

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24 pages, 1365 KiB  
Review
Bile Acids: Physiological Activity and Perspectives of Using in Clinical and Laboratory Diagnostics
by Yaroslav Shansky and Julia Bespyatykh
Molecules 2022, 27(22), 7830; https://doi.org/10.3390/molecules27227830 - 13 Nov 2022
Cited by 6 | Viewed by 2710
Abstract
Bile acids play a significant role in the digestion of nutrients. In addition, bile acids perform a signaling function through their blood-circulating fraction. They regulate the activity of nuclear and membrane receptors, located in many tissues. The gut microbiota is an important factor [...] Read more.
Bile acids play a significant role in the digestion of nutrients. In addition, bile acids perform a signaling function through their blood-circulating fraction. They regulate the activity of nuclear and membrane receptors, located in many tissues. The gut microbiota is an important factor influencing the effects of bile acids via enzymatic modification. Depending on the rate of healthy and pathogenic microbiota, a number of bile acids may support lipid and glucose homeostasis as well as shift to more toxic compounds participating in many pathological conditions. Thus, bile acids can be possible biomarkers of human pathology. However, the chemical structure of bile acids is similar and their analysis requires sensitive and specific methods of analysis. In this review, we provide information on the chemical structure and the biosynthesis of bile acids, their regulation, and their physiological role. In addition, the review describes the involvement of bile acids in various diseases of the digestive system, the approaches and challenges in the analysis of bile acids, and the prospects of their use in omics technologies. Full article
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