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Special Issue "Bioanalysis and Biological Matrix Sampling"

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

Deadline for manuscript submissions: 31 January 2021.

Special Issue Editors

Dr. Roberto Mandrioli
Website
Guest Editor
Department for Life Quality Studies, Alma Mater Studiorum – Università di Bologna, Rimini, Italy
Interests: drug analysis; toxicological analysis; HPLC; capillary electrophoresis; method development; microsampling; sample preparation; antioxidants; biological matrices
Special Issues and Collections in MDPI journals
Assoc. Prof. Dr. Laura Mercolini
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Guest Editor
Research group of Pharmaco-Toxicological Analysis (PTA Lab), Department of Pharmacy and Biotechnology (FaBiT), Alma Mater Studiorum - University of Bologna, Via Belmeloro 6, 40126 Bologna, Italy
Interests: bioanalysis; liquid chromatography; mass spectrometry; method validation; microsampling; sample treatment; central nervous system drugs; drugs of abuse; doping agents; natural products
Special Issues and Collections in MDPI journals
Dr. Michele Protti
Website
Guest Editor
Research group of Pharmaco-Toxicological Analysis (PTA Lab), Department of Pharmacy and Biotechnology (FaBiT), Alma Mater Studiorum - University of Bologna, Via Belmeloro 6, 40126 Bologna, Italy
Interests: HPLC; UHPLC; MS, HRMS; automation; biological matrix; miniaturized sample collection and preatreatment; CNS drugs; metabolites; biomarkers
Special Issues and Collections in MDPI journals

Special Issue Information

Dear Colleagues,

Bioanalysis is one of the most stimulating and complicated fields of analytical, medicinal, and biomedical chemistry. The high complexity of matrices coming from living beings is hardly matched, and most analytes, be they endogenous or exogenous, are found in these heterogeneous matrices at extremely low levels. The intrinsic instability and ease of degradation of biomatrices only adds to the difficulty of the endeavour.

As a consequence, bioanalysis requires cutting-edge levels of sensitivity, selectivity, reproducibility, and overall reliability together with top-level throughput. To tackle these challenges effectively, a huge array of sampling, sample preparation, and analysis combinations and workflows have been devised, tested, and applied.

The results have been nothing less than amazing. Material and instrumental advances, coupled to automation, miniaturisation, and to the ingenuity and expertise of thousands of researchers, have made this field one of the most advanced, attractive, and vibrant of all analytical chemistry.

In this Special Issue, we invite researchers to contribute innovative, original research articles and reviews papers related to the state of the art of all facets of biomatrix sampling, pretreatment, and analysis. Forensic, toxicological, anti-doping, and drug analyses are among the most important, but definitely not the only, aspects of the Special Issue. Proposals including all kinds of instrumental setups, endogenous and exogenous analytes, and biological matrices are welcome.

Potential topics include, but are not limited to the following:

  • Anti-doping analysis
  • Clinical analysis
  • Drug analysis
  • Forensic analysis
  • High-throughput or high-capacity analysis
  • Innovation in sampling
  • Sampling and microsampling
  • Toxicological analysis
  • Workflow and sample prep automation

Prof. Roberto Mandrioli
Prof. Dr. Laura Mercolini
Dr. Michele Protti
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 papers will be 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 2000 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

  • anti-doping
  • automation
  • bioanalysis
  • biological matrix
  • drug analysis
  • forensic analysis
  • sample preparation
  • sampling and microsampling
  • toxicological analysis

Published Papers (5 papers)

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Research

Open AccessArticle
Simultaneous Determination of Cortisol, Cortisone, and Multiple Illicit Drugs in Hair among Female Drug Addicts with LC-MS/MS
Molecules 2021, 26(2), 516; https://doi.org/10.3390/molecules26020516 - 19 Jan 2021
Abstract
Long-term dependence of illicit drugs impairs the function of the hypothalamic-pituitary-adrenal (HPA) axis, which regulates the secretion of endogenous steroids, cortisol, and cortisone. Thus, the present study aimed to develop a sensitive method for simultaneous determination of the multiple illicit drugs and two [...] Read more.
Long-term dependence of illicit drugs impairs the function of the hypothalamic-pituitary-adrenal (HPA) axis, which regulates the secretion of endogenous steroids, cortisol, and cortisone. Thus, the present study aimed to develop a sensitive method for simultaneous determination of the multiple illicit drugs and two steroids in hair to monitor the status of illicit drug exposure and the physiological and psychological health of drug addicts. The target analytes were extracted from hair by incubation with 1 mL methanol for 24 h at 40 °C and then determined with LC-APCI+-MS/MS. The validated method showed acceptable linearity (R2 > 0.99) in the range of 1.25–250 pg/mg for cortisol and cortisone, 2.5–125 pg/mg for heroin, 2.5–1250 pg/mg for ketamine, 2.5–5000 pg/mg for methamphetamine (MAM), 2.5–250 pg/mg for 3, 4-methylenedioxymethamphetamine (MDMA), morphine, and 6-monoacetylmorphine (6-AM). Limits of quantification were 1.6, 1.2, 1.6, 1.0, 1.4, 0.3, 2.1, and 1.2 pg/mg for cortisol, cortisone, heroin, ketamine, MAM, MDMA, morphine, and 6-AM, respectively. Method recoveries were from 90–115% for all analytes. Inter-day and intra-day coefficients of variation were within 10%. Finally, this method was successfully applied to detect the aforementioned analytes in hair among female drug addicts who self-reported to be MAM abuser, heroin abuser, ketamine abuser, and abuser of mixture drugs of MAM and heroin. MAM abusers with current MAM use showed significantly higher concentrations of cortisol, MAM, and MDMA than controls with drug withdrawal. Full article
(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)
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Open AccessArticle
LC-MS/MS Quantification of Nevirapine and Its Metabolites in Hair for Assessing Long-Term Adherence
Molecules 2020, 25(23), 5692; https://doi.org/10.3390/molecules25235692 - 02 Dec 2020
Abstract
The adherence assessment based on the combination of nevirapine (NVP) and its two metabolites (2-hydroxynevirapine and 3-hydroxynevirapine) would more comprehensively and accurately reflect long-term adherence than that of a single prototype. This study aimed to develop a specific, sensitive and selective method for [...] Read more.
The adherence assessment based on the combination of nevirapine (NVP) and its two metabolites (2-hydroxynevirapine and 3-hydroxynevirapine) would more comprehensively and accurately reflect long-term adherence than that of a single prototype. This study aimed to develop a specific, sensitive and selective method for simultaneous detection of the three compounds in hair and explore whether there was consistency among the three compounds in assessing long-term adherence. Furthermore, 75 HIV-positive patients who were taking the NVP drug were randomly recruited and divided into two groups (high-and low-adherence group). All participants self-reported their days of oral drug administration per month and provided their hair strands closest to the scalp at the region of posterior vertex. The concentrations of three compounds in the hair were determined using a developed LC-MS/MS method in multiple reaction monitoring. This method showed good performances in limit of quantification and accuracy with the recoveries from 85 to 115% and in precision with the intra-day and inter-day coefficients of variation within 15% for the three compounds. The population analysis revealed that patients with high-adherence showed significantly higher concentrations than those with low-adherence for all three compounds. There were significantly moderate correlations of nevirapine with 2-hydroxynevirapine and 3-hydroxynevirapin and high correlation between 2-hydroxynevirapine and 3-hydroxynevirapin. The two NVP’s metabolites showed high consistency with NVP in evaluating long-term adherence. Full article
(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)
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Open AccessArticle
Ultrasound–Vortex-Assisted Dispersive Liquid–Liquid Microextraction Combined with High Performance Liquid Chromatography–Diode Array Detection for Determining UV Filters in Cosmetics and the Human Stratum Corneum
Molecules 2020, 25(20), 4642; https://doi.org/10.3390/molecules25204642 - 12 Oct 2020
Abstract
This study explores the amounts of common chemical ultraviolet (UV) filters (i.e., avobenzone, bemotrizinol, ethylhexyl triazone, octocrylene, and octyl methoxycinnamate) in cosmetics and the human stratum corneum. An ultrasound–vortex-assisted dispersive liquid–liquid microextraction (US–VA–DLLME) method with a high-performance liquid chromatography–diode array detector was used [...] Read more.
This study explores the amounts of common chemical ultraviolet (UV) filters (i.e., avobenzone, bemotrizinol, ethylhexyl triazone, octocrylene, and octyl methoxycinnamate) in cosmetics and the human stratum corneum. An ultrasound–vortex-assisted dispersive liquid–liquid microextraction (US–VA–DLLME) method with a high-performance liquid chromatography–diode array detector was used to analyze UV filters. A bio-derived solvent (i.e., anisole) was used as the extractant in the US–VA–DLLME procedure, along with methanol as the dispersant, a vortexing time of 4 min, and ultrasonication for 3 min. The mass-transfer rate of the extraction process was enhanced due to vortex-ultrasound combination. Various C18 end-capped columns were used to investigate the separation characteristics of the UV filters, with XBridge BEH or CORTECS selected as the separation column. Calibration curves were constructed in the 0.05–5 μg/mL (all filters except octocrylene) and 0.1–10 μg/mL (octocrylene) ranges, and excellent analytical linearities with coefficients of determination (r2) above 0.998. The developed method was successfully used to analyze sunscreen. Moreover, experiments were designed to simulate the sunscreen-usage habits of consumers, and the cup method was used to extract UV filters from the human stratum corneum. The results suggest that a makeup remover should be employed to remove water-in-oil sunscreens from skin. Full article
(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)
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Open AccessArticle
Enhanced Extraction Technique of Omarigliptin from Human Plasma—Applied to Biological Samples from Healthy Human Volunteers
Molecules 2020, 25(18), 4232; https://doi.org/10.3390/molecules25184232 - 15 Sep 2020
Abstract
Enhancing drug extraction from human plasma is a challenging approach that critically affects pharmacokinetic and any further clinical studies based on the drug Cmin and Cmax values. It also has a serious impact on the sensitivity and the lower limit of [...] Read more.
Enhancing drug extraction from human plasma is a challenging approach that critically affects pharmacokinetic and any further clinical studies based on the drug Cmin and Cmax values. It also has a serious impact on the sensitivity and the lower limit of quantification (LLOQ) value of the bio-analytical methods. An advanced liquid chromatography tandem mass spectrometry (LC-MS/MS) bio-analytical method of omarigliptin (25–1000 nM) was established in human plasma using one-step liquid-liquid extraction. Alogliptin was used as an internal standard (IS) to attain good recovery and reproducibility while reducing the effects of the matrix. Enhanced plasma extraction of omarigliptin was successfully achieved with tertiary butyl methyl ether—diethyl ether (TBME-DEE) mixture as the extracting solvent, while using acetonitrile as the diluent solvent for the IS to effectively decrease the formed emulsion. Multiple Reaction Monitoring (MRM) of the transition pairs of m/z 399.2 to 153.0 for omarigliptin and m/z 340.2 to 116.0 for alogliptin was employed in positive Electro Spray Ionization (ESI) mode. Human plasma samples were collected after 1.5 h (tmax) of Marizev® (12.5 mg) tablets administration to healthy human volunteers showing average concentration of 292.18 nM. Validation results were all satisfactory including successful stability studies with bias below 12%. The proposed study will be valuable for ethnicity comparison studies that will be commenced on omarigliptin in Egypt by the authors in prospective study, following the FDA recommends, to evaluate possible sub-group dissimilarities that include pharmacokinetic parameters. Full article
(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)
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Open AccessFeature PaperArticle
Dried Urine Microsampling Coupled to Liquid Chromatography—Tandem Mass Spectrometry (LC–MS/MS) for the Analysis of Unconjugated Anabolic Androgenic Steroids
Molecules 2020, 25(14), 3210; https://doi.org/10.3390/molecules25143210 - 14 Jul 2020
Cited by 1
Abstract
Testing and monitoring anabolic androgenic steroids in biological fluids is a key activity in anti-doping practices. In this study, a novel approach is proposed, based on dried urine microsampling through two different workflows: dried urine spots (DUS) and volumetric absorptive microsampling (VAMS). Both [...] Read more.
Testing and monitoring anabolic androgenic steroids in biological fluids is a key activity in anti-doping practices. In this study, a novel approach is proposed, based on dried urine microsampling through two different workflows: dried urine spots (DUS) and volumetric absorptive microsampling (VAMS). Both techniques can overcome some common drawbacks of urine sampling, such as analyte instability and storage and transportation problems. Using an original, validated liquid chromatography–tandem mass spectrometry (LC-MS/MS) method, exogenous and endogenous unconjugated steroids were analysed. Despite the limitations of microsampling volume, good sensitivity was obtained (limit of quantitation ≤1.5 ng/mL for all analytes), with satisfactory precision (relative standard deviation <7.6%) and absolute recovery (>70.3%). Both microsampling platforms provide reliable results, in good agreement with those obtained from urine. Full article
(This article belongs to the Special Issue Bioanalysis and Biological Matrix Sampling)
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