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Separations
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Liquid Chromatography: Development of Separation Techniques
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Liquid Chromatography: Development of Separation Techniques

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Analysis of Natural Products and Pharmaceuticals".

Deadline for manuscript submissions: closed (25 December 2022) | Viewed by 9139

Special Issue Editor

Dr. Justyna Walczak-Skierska

E-Mail Website
Guest Editor
Interdisciplinary Centre for Modern Technologies, Nicolaus Copernicus University in Toruń, Wilenska 4, 87-100 Toruń, Poland
Interests: bioactive compounds; lipidomics; lipids; fatty acids; liquid chromatography; mass spectrometry
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Liquid chromatography is the most dynamically developing modern separation technique and is very widely used in the determination of both polar and non-polar compounds. The advantages of this technique include high efficiency, good resolution, high sensitivity, high process speed and the use of high pressures. These favorable parameters are achieved by introducing columns with small grains (1.7 μm). Due to the growing need to identify and determine more and more new analytes and metabolites in complex biological matrices, stationary phases with new fillings (e.g., imitating biological membranes), are used. Additionally, by miniaturization of the chromatographic columns, both the analysis time and the consumption of solvents are significantly reduced. In addition, the use of chemometric tools allows for the development of chromatographic conditions prior to injection.

Therefore, it is my pleasure to invite you to contribute your research article, communication, or review paper to this Special Issue dedicated to the development of new chromatographic methods in the analysis of biologically active compounds, natural products and drugs, the use of new stationary phases, and the modelling of chromatographic conditions.

Dr. Justyna Walczak-Skierska
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. Separations is an international peer-reviewed open access monthly 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 2600 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

  • liquid chromatography
  • stationary phases
  • mass spectrometry
  • natural product
  • drugs
  • retention mechanism
  • biologically active compounds

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Published Papers (3 papers)

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Research

14 pages, 909 KiB  
Article
Comparative Study of Various Procedures for Extracting Doxorubicin from Animal Tissue Samples
by Olga Maliszewska, Natalia Treder, Anna Roszkowska, Ilona Olędzka, Piotr Kowalski, Tomasz Bączek and Alina Plenis
Separations 2023, 10(1), 6; https://doi.org/10.3390/separations10010006 - 22 Dec 2022
Viewed by 2119
Abstract
This article presents a comparative study of selected deproteinization-, liquid–liquid-extraction- (LLE), and solid-phase-extraction (SPE)-based procedures for the isolation of doxorubicin (DOX) and daunorubicin (DAU) as an internal standard (IS) from rat tissue samples. During the experiments, all samples were analyzed via liquid chromatography [...] Read more.
This article presents a comparative study of selected deproteinization-, liquid–liquid-extraction- (LLE), and solid-phase-extraction (SPE)-based procedures for the isolation of doxorubicin (DOX) and daunorubicin (DAU) as an internal standard (IS) from rat tissue samples. During the experiments, all samples were analyzed via liquid chromatography coupled with fluorescence detection (LC-FL), with analytes being monitored at excitation and emission wavelengths of 487 and 555 nm, respectively. The absolute recoveries of the sample-preparation procedure were then calculated and compared, and the advantages and disadvantages of each approach were considered in depth. Ultimately, SPE with hydrophilic–lipophilic balanced (HLB) sorbents was selected as the most effective extraction procedure as it enabled the absolute recovery of DOX from tissue samples at a level of 91.6 ± 5.1%. Next, the selected HLB-SPE protocol was coupled with LC-FL separation and the resultant method was validated according to FDA and ICH requirements. The validation data confirmed that the developed procedure met all required criteria for bioanalytical methods, with a limit of detection (LOD) and limit of quantification (LOQ) of 0.005 µg/g and 0.01 µg/g, respectively. Finally, the developed protocol was successfully tested on various rat tissues enriched with DOX, confirming its potential as an interesting alternative to previously reported protocols for pharmacokinetic studies and clinical investigations aimed at analysis of the level and biodistribution of DOX in tissue samples after systemic administration of this drug. Full article
(This article belongs to the Special Issue Liquid Chromatography: Development of Separation Techniques)
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10 pages, 2564 KiB  
Article
Development of an Enzyme-Based Thin-Layer Chromatographic Assay for the Detection of Cyclooxygenase-2 Inhibitors
by Aurélie Urbain, Nidhal Trabelssi and Valérie Bardot
Separations 2022, 9(9), 238; https://doi.org/10.3390/separations9090238 - 2 Sep 2022
Cited by 2 | Viewed by 3775
Abstract
The search for new anti-inflammatory drugs with less side effects requires simple, fast and reliable screening methods. In this context, we have developed a sensitive thin-layer chromatographic (TLC) assay on silica gel plates to detect cyclooxygenase-2 (COX-2) inhibition. COX-2 catalyzes two sequential enzymatic [...] Read more.
The search for new anti-inflammatory drugs with less side effects requires simple, fast and reliable screening methods. In this context, we have developed a sensitive thin-layer chromatographic (TLC) assay on silica gel plates to detect cyclooxygenase-2 (COX-2) inhibition. COX-2 catalyzes two sequential enzymatic reactions: a first oxygenation step that converts arachidonic acid into prostaglandin G2, and a subsequent reduction of prostaglandin G2 into prostaglandin H2. Our test is based on the co-oxidation during this peroxidation step of a co-substrate, N,N,N′,N′-tetramethyl-p-phenylenediamine (TMPD), leading to a blue-grey product. As a consequence, COX-2 inhibitors appear on the TLC plate after revelation as clear spots against the colored background. Parameters such as concentrations of enzyme, substrate, and chromogenic reagent have been optimized. The limit of detection was found to be below the microgram for standard COX-2 inhibitors such as celecoxib or ibuprofen. The developed TLC assay was also conclusive when applied to 60 various natural pure compounds and some complex natural extracts. Results demonstrated a COX-2 inhibitory activity mostly for triterpene and sterol derivatives. This COX-2 TLC assay appears as a suitable low-cost and reliable strategy for the screening of natural extracts to discover new anti-inflammatory compounds. Full article
(This article belongs to the Special Issue Liquid Chromatography: Development of Separation Techniques)
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16 pages, 3042 KiB  
Article
Analysis of Major Polyphenolic Compounds of Cydonia oblonga Miller (Quince) Fruit Extract by UPLC-MS/MS and Its Effect on Adipogenesis in 3T3-L1 Cells
by Nawaz Khan, Nulibiya Maihemuti, Muhadaisi Nuer, Kayisaier Abudurousuli, Jimilihan Simayi, Ziruo Talihati, Mengyuan Han, Sendaer Hailati, Wenting Zhou and Ainiwaer Wumaier
Separations 2022, 9(7), 167; https://doi.org/10.3390/separations9070167 - 1 Jul 2022
Cited by 7 | Viewed by 2650
Abstract
Cydonia oblonga miller (quince) plant serves as a potential folk medicine for treating hypertension and cardiovascular diseases in China. However, to the best of our knowledge, no study has been conducted on the polyphenolic profile and anti-adipogenic effect of quince fruit grown in [...] Read more.
Cydonia oblonga miller (quince) plant serves as a potential folk medicine for treating hypertension and cardiovascular diseases in China. However, to the best of our knowledge, no study has been conducted on the polyphenolic profile and anti-adipogenic effect of quince fruit grown in China. In the current study, we aimed to investigate the quince fruit extract’s major phenolic compounds, evaluate their antioxidant activity, and examine their effect on adipogenesis in 3T3-L1 cells. A rapid and sensitive analytical method was established for the simultaneous determination of major polyphenolic compounds by using ultra-pressure liquid chromatography coupled with a triple quadrupole mass spectrometer (UPLC-MS/MS). Among the 10 compounds, the cryptochlorgenic acid was noticed as the most abundant compound of both purified (242.44 ± 0.73 µg/mg dw) and unpurified extract (3.37 ± 0.01 µg/mg dw) followed by quercetin 3-rutinoside and chlorogenic acid. Alternatively, both extracts possessed a high quantity of phenolic acids (purified extract = 483.10 ± 5.16 µg/mg dw and unpurified extract = 7.89 ± 0.02 µg/mg dw). The purified extract exhibited a strong antioxidant capacity (DPPH: EC50 = 3.316 µg/mL, ABTS: EC50 = 36.38 µg/mL) as compared to the unpurified extract. Additionally, our results also showed that the extract at 100 µg/mL significantly suppressed the preadipocyte differentiation and decreased the lipid droplets up to 69% in mature adipocytes. The present study highlights an accurate and fast detection method for quince fruit extract polyphenolic compounds with its antioxidant and antiadipogenic effects. The study also provides the necessary information for the rational development and utilization of quince fruit extract as a source of phytochemicals. Full article
(This article belongs to the Special Issue Liquid Chromatography: Development of Separation Techniques)
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