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Analysis of Drugs and Biologically Active Compounds Using Chromatographic and...
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Analysis of Drugs and Biologically Active Compounds Using Chromatographic and Electromigration Techniques

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

Deadline for manuscript submissions: closed (31 October 2021) | Viewed by 23550

Special Issue Editors

Prof. Dr. Ewa Kłodzińska

E-Mail Website
Guest Editor
Department of Analytical Chemistry and Instrumental Analysis, Institute of Sport-National Research Institute, Warsaw, Poland
Interests: electromigration techniques; bacteria characterization by capillary electrophoresis; wound dressing; zeta potential measurements; drug release from biomaterials
Special Issues, Collections and Topics in MDPI journals
Dr. Muhammad Ajmal Shah

E-Mail Website
Assistant Guest Editor
Department of Pharmacy, Hazara University, Mansehra, Pakistan
Interests: green extraction and enrichement of biaoctive compounds; nutraceuticals; antidiabetic; antidiabesitic; neuroprotection; anti-Alzheimer; anti-Parkinson’s
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Analysis of biologically active substances is particularly important in the pharmaceutical and biomedical area. The chemical compounds which are present in the environment usually cause bad effects on health, the most serious ones being tumors and various mutations on a cellular level. Those compounds, from an analytical point of view, can serve the function of biomarkers, constituting measurable changes in the organism’s cells and biochemical processes occurring therein. The challenge of the 21st century is therefore finding effective and reliable methods of identification of biomarkers as well as understanding bodily functions, which occur in living organisms on a molecular level. 

On the other hand, the detection and deterrence of abuse of performance-enhancing drugs in sport and also determination of the chemical composition of dietary supplements are important for maintaining a level playing field among athletes and for decreasing the threat to athletes’ health. Among the classes of prohibited substances (WADA prohibited list), three have given rise to the most recent analytical developments in the field: anabolic agents; peptide and protein hormones; and methods to increase oxygen delivery to tissues, including recombinant erythropoietin. Methods for anabolic agents, including designer steroids, have been enhanced through the use of chromatography coupled with mass spectrometry (GC/MS, LC/MS) and also electromigration techniques (CZE, MEKC). Incorporation of techniques such as flow cytometry, isoelectric focusing, and zeta potential measurements have supported the detection of blood doping. 

The aim of this Special Issue is to cover topics related to the simulation determination of biologically active compounds (drugs, dietary supplements, biomarkers, doping substances) in biological samples and pharmaceutical products and the application of proposed analytical methods in medical diagnosis, antidoping research, and also pharmaceutical and biomedical area.  

Real applications addressing dietary supplements, drugs, food, and biological and environmental systems are welcome. Researchers are cordially invited to contribute with original research and review articles to this Special Issue.

Prof. Dr. Ewa Kłodzińska
Guest Editor

Dr. Muhammad Ajmal Shah
Assistant Guest Editor

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

  • Analytical chemistry
  • Chromatography
  • Electromigration techniques
  • Biomarkers
  • Medical diagnosis
  • Zeta potential measurements
  • Determination of doping substances and dietary supplements

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Published Papers (5 papers)

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Research

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13 pages, 1186 KiB  
Article
HPLC Analysis of the Urinary Iodine Concentration in Pregnant Women
by Aniceta A. Mikulska, Dorota Filipowicz, Franciszek K. Główka, Ewelina Szczepanek-Parulska, Marek Ruchała, Michał Bartecki and Marta Karaźniewicz-Łada
Molecules 2021, 26(22), 6797; https://doi.org/10.3390/molecules26226797 - 10 Nov 2021
Cited by 5 | Viewed by 3140
Abstract
Iodine is an essential component for fetal neurodevelopment and maternal thyroid function. Urine iodine is the most widely used indicator of iodine status. In this study, a novel validated ion-pair HPLC–UV method was developed to measure iodine concentration in clinical samples. A sodium [...] Read more.
Iodine is an essential component for fetal neurodevelopment and maternal thyroid function. Urine iodine is the most widely used indicator of iodine status. In this study, a novel validated ion-pair HPLC–UV method was developed to measure iodine concentration in clinical samples. A sodium thiosulfate solution was added to the urine sample to convert the total free iodine to iodide. Chromatographic separation was achieved in a Pursuit XRs C8 column. The mobile phase consisted of acetonitrile and a water phase containing 18-crown-6-ether, octylamine and sodium dihydrogen phosphate. Validation parameters, such as accuracy, precision, limits of detection and quantification, linearity and stability, were determined. Urinary samples from pregnant women were used to complete the validation and confirm the method’s applicability. In the studied population of 93 pregnant women, the median UIC was lower in the group without iodine supplementation (117 µg/L, confidence interval (%CI): 95; 138) than in the supplement group (133 µg/L, %CI: 109; 157). In conclusion, the newly established ion-pair HPLC–UV method was adequately precise, accurate and fulfilled validation the criteria for analyzing compounds in biological fluids. The method is less complicated and expensive than other frequently used assays and permits the identification of the iodine-deficient subjects. Full article
(This article belongs to the Special Issue Analysis of Drugs and Biologically Active Compounds Using Chromatographic and Electromigration Techniques)
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19 pages, 6341 KiB  
Article
Keratin Scaffolds Containing Casomorphin Stimulate Macrophage Infiltration and Accelerate Full-Thickness Cutaneous Wound Healing in Diabetic Mice
by Marek Konop, Anna K. Laskowska, Mateusz Rybka, Ewa Kłodzińska, Dorota Sulejczak, Robert A. Schwartz and Joanna Czuwara
Molecules 2021, 26(9), 2554; https://doi.org/10.3390/molecules26092554 - 27 Apr 2021
Cited by 18 | Viewed by 4267
Abstract
Impaired wound healing is a major medical challenge, especially in diabetics. Over the centuries, the main goal of tissue engineering and regenerative medicine has been to invent biomaterials that accelerate the wound healing process. In this context, keratin-derived biomaterial is a promising candidate [...] Read more.
Impaired wound healing is a major medical challenge, especially in diabetics. Over the centuries, the main goal of tissue engineering and regenerative medicine has been to invent biomaterials that accelerate the wound healing process. In this context, keratin-derived biomaterial is a promising candidate due to its biocompatibility and biodegradability. In this study, we evaluated an insoluble fraction of keratin containing casomorphin as a wound dressing in a full-thickness surgical skin wound model in mice (n = 20) with iatrogenically induced diabetes. Casomorphin, an opioid peptide with analgesic properties, was incorporated into keratin and shown to be slowly released from the dressing. An in vitro study showed that keratin-casomorphin dressing is biocompatible, non-toxic, and supports cell growth. In vivo experiments demonstrated that keratin-casomorphin dressing significantly (p < 0.05) accelerates the whole process of skin wound healing to the its final stage. Wounds covered with keratin-casomorphin dressing underwent reepithelization faster, ending up with a thicker epidermis than control wounds, as confirmed by histopathological and immunohistochemical examinations. This investigated dressing stimulated macrophages infiltration, which favors tissue remodeling and regeneration, unlike in the control wounds in which neutrophils predominated. Additionally, in dressed wounds, the number of microhemorrhages was significantly decreased (p < 0.05) as compared with control wounds. The dressing was naturally incorporated into regenerating tissue during the wound healing process. Applied keratin dressing favored reconstruction of more regular skin structure and assured better cosmetic outcome in terms of scar formation and appearance. Our results have shown that insoluble keratin wound dressing containing casomorphin supports skin wound healing in diabetic mice. Full article
(This article belongs to the Special Issue Analysis of Drugs and Biologically Active Compounds Using Chromatographic and Electromigration Techniques)
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10 pages, 1249 KiB  
Article
The Double Face of Ketamine—The Possibility of Its Identification in Blood and Beverages
by Magdalena Świądro, Paweł Stelmaszczyk, Irena Lenart and Renata Wietecha-Posłuszny
Molecules 2021, 26(4), 813; https://doi.org/10.3390/molecules26040813 - 4 Feb 2021
Cited by 8 | Viewed by 3401
Abstract
The purpose of this study was to develop and validate a high-sensitivity methodology for identifying one of the most used drugs—ketamine. Ketamine is used medicinally to treat depression, alcoholism, and heroin addiction. Moreover, ketamine is the main ingredient used in so-called “date-rape” pills [...] Read more.
The purpose of this study was to develop and validate a high-sensitivity methodology for identifying one of the most used drugs—ketamine. Ketamine is used medicinally to treat depression, alcoholism, and heroin addiction. Moreover, ketamine is the main ingredient used in so-called “date-rape” pills (DRP). This study presents a novel methodology for the simultaneous determination of ketamine based on the Dried Blood Spot (DBS) method, in combination with capillary electrophoresis coupled with a mass spectrometer (CE-TOF-MS). Then, 6-mm circles were punched out from DBS collected on Whatman DMPK-C paper and extracted using microwave-assisted extraction (MAE). The assay was linear in the range of 25–300 ng/mL. Values of limits of detection (LOD = 6.0 ng/mL) and quantification (LOQ = 19.8 ng/mL) were determined based on the signal to noise ratio. Intra-day precision at each determined concentration level was in the range of 6.1–11.1%, and inter-day between 7.9–13.1%. The obtained precision was under 15.0% (for medium and high concentrations) and lower than 20.0% (for low concentrations), which are in accordance with acceptance criteria. Therefore, the DBS/MAE/CE-TOF-MS method was successfully checked for analysis of ketamine in matrices other than blood, i.e., rose wine and orange juice. Moreover, it is possible to identify ketamine in the presence of flunitrazepam, which is the other most popular ingredient used in DRP. Based on this information, the selectivity of the proposed methodology for identifying ketamine in the presence of other components of rape pills was checked. Full article
(This article belongs to the Special Issue Analysis of Drugs and Biologically Active Compounds Using Chromatographic and Electromigration Techniques)
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14 pages, 1530 KiB  
Article
Development and Optimization of a High Sensitivity LC-MS/MS Method for the Determination of Hesperidin and Naringenin in Rat Plasma: Pharmacokinetic Approach
by Jesús Alfredo Araujo-León, Rolffy Ortiz-Andrade, Rivelino Armando Vera-Sánchez, Julio Enrique Oney-Montalvo, Tania Isolina Coral-Martínez and Zulema Cantillo-Ciau
Molecules 2020, 25(18), 4241; https://doi.org/10.3390/molecules25184241 - 16 Sep 2020
Cited by 14 | Viewed by 3595
Abstract
The purpose of this study was to develop, optimize, and fully validate a high-sensitivity methodology using UHPLC-MS/MS to simultaneously quantify hesperidin and naringenin in microsamples (100 µL) of murine plasma after intragastric administration of single pure flavonoids and a mixture. The optimization process [...] Read more.
The purpose of this study was to develop, optimize, and fully validate a high-sensitivity methodology using UHPLC-MS/MS to simultaneously quantify hesperidin and naringenin in microsamples (100 µL) of murine plasma after intragastric administration of single pure flavonoids and a mixture. The optimization process allowed for high sensitivity with detection limits of approximately picogram order using an electrospray ionization (ESI) source in negative mode and an experiment based on multiple reaction monitoring (MRM). The validation parameters showed excellent linearity and detection limits, with a precision of less than 8% and a recovery of over 90%. This methodology was applied to compare the pharmacokinetic parameters for the administration of hesperidin and naringenin in individual form or in the form of a mixture. The results showed an absence of significant effects (p > 0.05) for Tmax and Cmax; however, the AUC presented significant differences (p < 0.05) for both flavonoids when administered as a mixture, showing an improved absorption ratio for both flavonoids. Full article
(This article belongs to the Special Issue Analysis of Drugs and Biologically Active Compounds Using Chromatographic and Electromigration Techniques)
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Review

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26 pages, 529 KiB  
Review
Recent Materials Developed for Dispersive Solid Phase Extraction
by Piotr Ścigalski and Przemysław Kosobucki
Molecules 2020, 25(21), 4869; https://doi.org/10.3390/molecules25214869 - 22 Oct 2020
Cited by 65 | Viewed by 7174
Abstract
Solid phase extraction (SPE) is an analytical procedure developed with the purpose of separating a target analyte from a complex sample matrix prior to quantitative or qualitative determination. The purpose of such treatment is twofold: elimination of matrix constituents that could interfere with [...] Read more.
Solid phase extraction (SPE) is an analytical procedure developed with the purpose of separating a target analyte from a complex sample matrix prior to quantitative or qualitative determination. The purpose of such treatment is twofold: elimination of matrix constituents that could interfere with the detection process or even damage analytical equipment as well as enriching the analyte in the sample so that it is readily available for detection. Dispersive solid phase extraction (dSPE) is a recent development of the standard SPE technique that is attracting growing attention due to its remarkable simplicity, short extraction time and low requirement for solvent expenditure, accompanied by high effectiveness and wide applicability. This review aims to thoroughly survey recently conducted analytical studies focusing on methods utilizing novel, interesting nanomaterials as dSPE sorbents, as well as known materials that have been only recently successfully applied in dSPE techniques, and evaluate their performance and suitability based on comparison with previously reported analytical procedures. Full article
(This article belongs to the Special Issue Analysis of Drugs and Biologically Active Compounds Using Chromatographic and Electromigration Techniques)
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