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Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics,...
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Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest

A special issue of Pharmaceuticals (ISSN 1424-8247). This special issue belongs to the section "Natural Products".

Deadline for manuscript submissions: closed (31 August 2023) | Viewed by 30684

Printed Edition Available!
A printed edition of this Special Issue is available here.

Special Issue Editors

Prof. Dr. Jan Oszmianski

E-Mail Website
Guest Editor
Retired Professor, Wrocław, Poland
Interests: phenolic compounds; isolation and qualitative and quantitative determination of polyphenols; bioactive compounds; UV-VIS HPLC-MS-MS and SPE
Special Issues, Collections and Topics in MDPI journals
Dr. Sabina Lachowicz-Wiśniewska

E-Mail Website
Guest Editor
Faculty of Health Sciences, Department Food and Nutrition, Calisia University, 4 Nowy Świat Street, 62-800 Kalisz, Poland
Interests: nutraceuticals and functional foods; medicinal plants; bioactive compounds; HPLC; LC-MS; nutrition; antioxidant agent; prebiotics; probiotics; symbiotics; bioavailability in vitro
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

It is our pleasure to present this Special Issue of Pharmaceuticals, entitled “Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest”. Plants produce a wide range of phytochemicals, known as non-nutrition compounds, in order to confirm their identity and they are used for the production of natural pharmaceuticals, cosmetics, functional food, among other things due to the pro-health properties. The use of modern chromatographic techniques allows for accurate quantitative and qualitative identification of the above-mentioned phytochemicals and their natural products. Liquid chromatography is one of the most efficient and robust specific techniques, due to the merits of convenience and strong separation ability, as well as a wide range of material applications for identification. Liquid chromatography is widely used for the analysis of plants, nutraceuticals, pharmaceuticals, cosmetics, natural product quality control, or quantitative determination of bioactive compounds. The most commonly used for the identification of different plant material and pharmaceuticals are the ultra- and high-performance liquid chromatography with UV-VIS, fluorescence, diode array, and are equipped with mass spectrometry or tandem mass spectrometry detection methods. Therefore, for this Special Issue, we will publish studies concerning the latest scientific news, insights, and advances in the field of innovation of liquid chromatography for the analysis of bioactive compounds for pharmaceuticals, cosmetics, and functional food interest. Original research articles, short communications, and critical review articles dealing with extraction and identification of bioactive compounds from natural matrices with biological and pharmaceutical interest ​are welcome. The information presented will certainly arouse considerable interest among a large group of our readers from different disciplines and research fields.

Prof. Dr. Jan Oszmianski
Dr. Sabina Lachowicz-Wiśniewska
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. Pharmaceuticals 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 2900 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

  • plant materials
  • pharmaceuticals
  • product quality
  • innovative methods
  • polyphenolic compounds
  • isoprenoids
  • bioactive compounds
  • food chemistry
  • natural products
  • mass spectrometry
  • extraction
  • LC-MS/MS techniques
  • HPLC-DAD-MS

Published Papers (17 papers)

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Research

20 pages, 6018 KiB  
Article
Optimisation of Solid-Phase Extraction and LC-MS/MS Analysis of Six Breast Cancer Drugs in Patient Plasma Samples
by Lu Turković, Dragana Mutavdžić Pavlović, Zvonimir Mlinarić, Anamarija Skenderović, Tajana Silovski and Miranda Sertić
Pharmaceuticals 2023, 16(10), 1445; https://doi.org/10.3390/ph16101445 - 12 Oct 2023
Cited by 1 | Viewed by 1204
Abstract
In the development of bioanalytical LC-MS methods for the determination of drugs in plasma samples in a clinical setting, adequate sample preparation is of utmost importance. The main goals are to achieve the selective extraction of the analytes of interest and attain thorough [...] Read more.
In the development of bioanalytical LC-MS methods for the determination of drugs in plasma samples in a clinical setting, adequate sample preparation is of utmost importance. The main goals are to achieve the selective extraction of the analytes of interest and attain thorough matrix removal while retaining acceptable ecological properties, cost-effectiveness, and high throughput. Solid-phase extraction (SPE) offers a versatile range of options, from the selection of an appropriate sorbent to the optimisation of the washing and elution conditions. In this work, the first SPE method for the simultaneous extraction of six anticancer drugs used in novel therapeutic combinations for advanced breast cancer treatment—palbociclib, ribociclib, abemaciclib, anastrozole, letrozole, and fulvestrant—was developed. The following sorbent chemistries were tested: octylsilyl (C8), octadecylsilyl (C18), hydrophilic–lipophilic balance (HLB), mixed-mode cation-exchange (MCX and X-C), and mixed-mode weak cation-exchange (WCX), with different corresponding elution solvents. The samples were analysed using LC-MS/MS, with a phenyl column (150 × 4.6 mm, 2.5 μm). The best extraction recoveries (≥92.3%) of all analytes were obtained with the C8 phase, using methanol as the elution solvent. The optimised method was validated in the clinically relevant ranges, showing adequate precision (inter-day RSD ≤ 14.3%) and accuracy (inter-day bias −12.7–13.5%). Finally, its applicability was successfully proven by the analysis of samples from breast cancer patients. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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17 pages, 3044 KiB  
Article
Study of Mono and Di-O-caffeoylquinic Acid Isomers in Acmella oleracea Extracts by HPLC-MS/MS and Application of Linear Equation of Deconvolution Analysis Algorithm for Their Characterization
by Maria Bellumori, Marco Pallecchi, Beatrice Zonfrillo, Luigi Lucio, Marta Menicatti, Marzia Innocenti, Nadia Mulinacci and Gianluca Bartolucci
Pharmaceuticals 2023, 16(10), 1375; https://doi.org/10.3390/ph16101375 - 28 Sep 2023
Cited by 1 | Viewed by 656
Abstract
Chlorogenic acids, the esters of caffeic and quinic acids, are the main phenolic acids detected in Acmella oleracea extracts and have gained increasing interest in recent years due to their important biological activities. Given their structural similarity and instability, the correct analysis and [...] Read more.
Chlorogenic acids, the esters of caffeic and quinic acids, are the main phenolic acids detected in Acmella oleracea extracts and have gained increasing interest in recent years due to their important biological activities. Given their structural similarity and instability, the correct analysis and identification of these compounds in plants is challenging. This study aimed to propose a simple and rapid determination of the A. oleracea caffeoylquinic isomers, applying an HPLC-MS/MS method supported by a mathematical algorithm (Linear Equation of Deconvolution Analysis (LEDA)). The three mono- and the three di-caffeoylquinic acids in roots of Acmella plants were studied by an ion trap MS analyzer. A separation by a conventional chromatographic method was firstly performed and an MS/MS characterization by energetic dimension of collision-induced dissociation mechanism was carried out. The analyses were then replicated using a short HPLC column and a fast elution gradient (ten minutes). Each acquired MS/MS data were processed by LEDA algorithm which allowed to assign a relative abundance in the reference ion signal to each isomer present. Quantitative results showed no significant differences between the two chromatographic systems proposed, proving that the use of LEDA algorithm allowed the distinction of the six isomers in a quarter of the time. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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18 pages, 6970 KiB  
Article
Unraveling the Radioprotective Mechanisms of UV-Resistant Bacillus subtilis ASM-1 Extracted Compounds through Molecular Docking
by Asim Ur Rahman, Aftab Ali, Faisal Ahmad, Sajjad Ahmad, Metab Alharbi, Abdullah F. Alasmari, Amna Fayyaz, Qurrat ul ain Rana, Samiullah Khan, Fariha Hasan, Malik Badshah and Aamer Ali Shah
Pharmaceuticals 2023, 16(8), 1139; https://doi.org/10.3390/ph16081139 - 11 Aug 2023
Viewed by 912
Abstract
Radioresistant microorganisms possess inimitable capabilities enabling them to thrive under extreme radiation. However, the existence of radiosensitive microorganisms inhabiting such an inhospitable environment is still a mystery. The current study examines the potential of radioresistant microorganisms to protect radiosensitive microorganisms in harsh environments. [...] Read more.
Radioresistant microorganisms possess inimitable capabilities enabling them to thrive under extreme radiation. However, the existence of radiosensitive microorganisms inhabiting such an inhospitable environment is still a mystery. The current study examines the potential of radioresistant microorganisms to protect radiosensitive microorganisms in harsh environments. Bacillus subtilis strain ASM-1 was isolated from the Thal desert in Pakistan and evaluated for antioxidative and radioprotective potential after being exposed to UV radiation. The strain exhibited 54.91% survivability under UVB radiation (5.424 × 103 J/m2 for 8 min) and 50.94% to mitomycin-C (4 µg/mL). Extracellular fractions collected from ASM-1 extracts showed significant antioxidant potential, and chemical profiling revealed a pool of bioactive compounds, including pyrrolopyrazines, amides, alcoholics, and phenolics. The E-2 fraction showed the maximum antioxidant potential via DPPH assay (75%), and H2O2 scavenging assay (68%). A combination of ASM-1 supernatant with E-2 fraction (50 µL in a ratio of 2:1) provided substantial protection to radiosensitive cell types, Bacillus altitudinis ASM-9 (MT722073) and E. coli (ATCC 10536), under UVB radiation. Docking studies reveal that the compound supported by literature against the target proteins have strong binding affinities which further inferred its medical uses in health care treatment. This is followed by molecular dynamic simulations where it was observed among trajectories that there were no significant changes in major secondary structure elements, despite the presence of naturally flexible loops. This behavior can be interpreted as a strategy to enhance intermolecular conformational stability as the simulation progresses. Thus, our study concludes that Bacillus subtilis ASM-1 protects radiosensitive strains from radiation-induced injuries via biofilm formation and secretion of antioxidative and radioprotective compounds in the environment. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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15 pages, 2646 KiB  
Article
Bioanalytical LC-QTOF/MS Method for a N-phenylpiperazine Derivate (LQFM05): An Anxiolytic- and Antidepressant-like Prototype Drug Applied to Pharmacokinetic and Biodistribution Studies
by Ana Cláudia M. Ramos, Kênnia R. Rezende, Carolina M. Teixeira, Aline R. Fernandes, Heloa Santos, Rúbia Darc Machado, Ricardo Menegatti, Boniek G. Vaz and Andréa R. Chaves
Pharmaceuticals 2023, 16(7), 930; https://doi.org/10.3390/ph16070930 - 26 Jun 2023
Cited by 3 | Viewed by 1389
Abstract
The LQFM05 is a prototype drug designed for treatment of psychiatric disorders, such as schizophrenia, exhibiting anxiolytic- and antidepressant-like (12 or 24 µmol/kg) effects in classical behavioral tests. In order to evaluate its pharmacokinetic properties, a liquid chromatography method coupled to a quadrupole [...] Read more.
The LQFM05 is a prototype drug designed for treatment of psychiatric disorders, such as schizophrenia, exhibiting anxiolytic- and antidepressant-like (12 or 24 µmol/kg) effects in classical behavioral tests. In order to evaluate its pharmacokinetic properties, a liquid chromatography method coupled to a quadrupole time of flight mass spectrometry system (LC-QTOF/MS) was developed and fully validated for LQFM05 analysis in rat plasma and tissue samples (brain, heart, liver, and kidneys). Liquid–liquid extraction, solid phase extraction and protein precipitation were assessed as clean-up procedures for biological samples and analyte enrichment. Plasma and tissue samples underwent protein precipitation as a preliminary step, using acetonitrile. Linearity was fully demonstrated for the dynamic range (10.0 to 900.0 ng/mL), with r2 values higher than 0.99 (RSDslope ≤ 2%, Fcal < Ftab, Ccal < Ctab). Biodistribution studies in rats revealed high brain tissue concentrations (12.4 µg/g), suggesting elevated drug affinity to the main therapeutic target tissue, showing a blood partition coefficient of 1.9. Kidneys also showed great exposure and tissue affinity, suggesting a potential extrahepatic clearance. Likewise, all examined tissues exhibited satisfactory LQFMF05 distribution. The mass fragmentation spectrum indicated the presence of its main metabolite, LQFM235, yielded by high hepatic hydroxylation route, an equally bioactive derivative. Lastly, the developed LC-QTOF/MS method was shown to be sensitive (LOQ = 10 ng/mL), precise and accurate for LQFM05 determination in tissue homogenates and plasma samples. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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14 pages, 1046 KiB  
Article
A Novel UHPLC-MS/MS Method for the Quantification of Seven Opioids in Different Human Tissues
by Alessandra Manca, Amedeo De Nicolò, Elisa Delia De Vivo, Micol Ferrara, Sharon Oh, Sahar Khalili, Niamh Higgins, Robert G. Deiss, Stefano Bonora, Jessica Cusato, Alice Palermiti, Jacopo Mula, Sara Gianella and Antonio D’Avolio
Pharmaceuticals 2023, 16(6), 903; https://doi.org/10.3390/ph16060903 - 19 Jun 2023
Viewed by 1685
Abstract
Background: Opioids are considered the cornerstone of pain management: they show good efficacy as a first-line therapy for moderate to severe cancer pain. Since pharmacokinetic/pharmacodynamic information about the tissue-specific effect and toxicity of opioids is still scarce, their quantification in post-mortem autoptic specimens [...] Read more.
Background: Opioids are considered the cornerstone of pain management: they show good efficacy as a first-line therapy for moderate to severe cancer pain. Since pharmacokinetic/pharmacodynamic information about the tissue-specific effect and toxicity of opioids is still scarce, their quantification in post-mortem autoptic specimens could give interesting insights. Methods: We describe an ultra-high-performance liquid chromatography coupled with tandem mass spectrometry method for the simultaneous quantification of methadone, morphine, oxycodone, hydrocodone, oxymorphone, hydromorphone and fentanyl in several tissues: liver, brain, kidney, abdominal adipose tissue, lung and blood plasma. The presented method has been applied on 28 autoptic samples from different organs obtained from four deceased PLWH who used opioids for palliative care during terminal disease. Results: Sample preparation was based on tissue weighing, disruption, sonication with drug extraction medium and a protein precipitation protocol. The extracts were then dried, reconstituted and injected onto the LX50 QSight 220 (Perkin Elmer, Milan, Italy) system. Separation was obtained by a 7 min gradient run at 40 °C with a Kinetex Biphenyl 2.6 µm, 2.1 × 100 mm. Concerning the analyzed samples, higher opioids concentrations were observed in tissues than in plasma. Particularly, O-MOR and O-COD showed higher concentrations in kidney and liver than other tissues (>15–20 times greater) and blood plasma (>100 times greater). Conclusions: Results in terms of linearity, accuracy, precision, recovery and matrix effect fitted the recommendations of FDA and EMA guidelines, and the sensitivity was high enough to allow successful application on human autoptic specimens from an ethically approved clinical study, confirming its eligibility for post-mortem pharmacological/toxicological studies. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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17 pages, 2877 KiB  
Article
Application of Direct Thermal Desorption–Gas Chromatography–Mass Spectrometry for Determination of Volatile and Semi-Volatile Organosulfur Compounds in Onions: A Novel Analytical Approach
by Ana V. González-de-Peredo, Mercedes Vázquez-Espinosa, Estrella Espada-Bellido, Marta Ferreiro-González, Ceferino Carrera, Miguel Palma and Gerardo F. Barbero
Pharmaceuticals 2023, 16(5), 715; https://doi.org/10.3390/ph16050715 - 08 May 2023
Cited by 1 | Viewed by 1387
Abstract
The population is now more aware of their diets due to the connection between food and general health. Onions (Allium cepa L.), common vegetables that are minimally processed and grown locally, are known for their health-promoting properties. The organosulfur compounds present in [...] Read more.
The population is now more aware of their diets due to the connection between food and general health. Onions (Allium cepa L.), common vegetables that are minimally processed and grown locally, are known for their health-promoting properties. The organosulfur compounds present in onions have powerful antioxidant properties and may decrease the likelihood of developing certain disorders. It is vital to employ an optimum approach with the best qualities for studying the target compounds to undertake a thorough analysis of these compounds. In this study, the use of a direct thermal desorption–gas chromatography–mass spectrometry method with a Box–Behnken design and multi-response optimization is proposed. Direct thermal desorption is an environmentally friendly technique that eliminates the use of solvents and requires no prior preparation of the sample. To the author’s knowledge, this methodology has not been previously used to study the organosulfur compounds in onions. Likewise, the optimal conditions for pre-extraction and post-analysis of organosulfur compounds were as follows: 46 mg of onion in the tube, a desorption heat of 205 °C for 960 s, and a trap heat of 267 °C for 180 s. The repeatability and intermediate precision of the method were evaluated by conducting 27 tests over three consecutive days. The results obtained for all compounds studied revealed CV values ranging from 1.8% to 9.9%. The major compound reported in onions was 2,4-dimethyl-thiophene, representing 19.4% of the total area of sulfur compounds. The propanethial S-oxide, the principal compound responsible for the tear factor, accounted for 4.5% of the total area. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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28 pages, 5158 KiB  
Article
Identification of Compounds of Crocus sativus by GC-MS and HPLC/UV-ESI-MS and Evaluation of Their Antioxidant, Antimicrobial, Anticoagulant, and Antidiabetic Properties
by Aziz Drioiche, Atika Ailli, Nadia Handaq, Firdaous Remok, Mohamed Elouardi, Hajar Elouadni, Omkulthom Al Kamaly, Asmaa Saleh, Mohamed Bouhrim, Hanane Elazzouzi, Fadoua El Makhoukhi and Touriya Zair
Pharmaceuticals 2023, 16(4), 545; https://doi.org/10.3390/ph16040545 - 05 Apr 2023
Cited by 4 | Viewed by 2427
Abstract
In order to valorize the species Crocus sativus from Morocco and to prepare new products with high added value that can be used in the food and pharmaceutical industry, our interest was focused on the phytochemical characterization and the biological and pharmacological properties [...] Read more.
In order to valorize the species Crocus sativus from Morocco and to prepare new products with high added value that can be used in the food and pharmaceutical industry, our interest was focused on the phytochemical characterization and the biological and pharmacological properties of the stigmas of this plant. For this purpose, the essential oil of this species, extracted by hydrodistillation and then analyzed by GC-MS, revealed a predominance of phorone (12.90%); (R)-(-)-2,2-dimethyl-1,3-dioxolane-4-methanol (11.65%); isopropyl palmitate (9.68%); dihydro-β-ionone (8.62%); safranal (6.39%); trans-β-ionone (4.81%); 4-keto-isophorone (4.72%); and 1-eicosanol (4.55%) as the major compounds. The extraction of phenolic compounds was performed by decoction and Soxhlet extraction. The results of the determination of flavonoids, total polyphenols, condensed tannins, and hydrolyzable tannins determined by spectrophotometric methods on aqueous and organic extracts have proved the richness of Crocus sativus in phenolic compounds. Chromatographic analysis by HPLC/UV-ESI-MS of Crocus sativus extracts revealed the presence of crocin, picrocrocin, crocetin, and safranal molecules specific to this species. The study of antioxidant activity by three methods (DPPH, FRAP, and total antioxidant capacity) has proved that C. sativus is a potential source of natural antioxidants. Antimicrobial activity of the aqueous extract (E0) was investigated by microdilution on a microplate. The results have revealed the efficacy of the aqueous extract against Acinetobacter baumannii and Shigella sp. with MIC ≤ 600 µg/mL and against Aspergillus niger, Candida kyfer, and Candida parapsilosis with MIC = 2500 µg/mL. Measurements of pro-thrombin time (PT) and activated partial thromboplastin time (aPTT) in citrated plasma obtained from routine healthy blood donors were used to determine the anticoagulant activity of aqueous extract (E0). The anticoagulant activity of the extract (E0) studied showed that this extract can significantly prolong the partial thromboplastin time (p < 0.001) with a 359 µg/mL concentration. The antihyperglycemic effect of aqueous extract was studied in albino Wistar rats. The aqueous extract (E0) showed strong in vitro inhibitory activity of α-amylase and α-glucosidase compared with acarbose. Thus, it very significantly inhibited postprandial hyperglycemia in albino Wistar rats. According to the demonstrated results, we can affirm the richness of Crocus sativus stigmas in bioactive molecules and its use in traditional medicine. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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14 pages, 2477 KiB  
Article
Analysis of Transfer of Tiamulin to Animal Tissue after Oral Administration: An Important Factor for Ensuring Food Safety and Environmental Protection
by Viviana Carmen Ciucă, Carmen Otilia Rusănescu and Victor Viorel Safta
Pharmaceuticals 2023, 16(3), 387; https://doi.org/10.3390/ph16030387 - 02 Mar 2023
Cited by 3 | Viewed by 1496
Abstract
The administration of veterinary medicinal products containing tiamulin hydrogen fumarate (THF) leads to the appearance of the following residues in animal tissues: THF and metabolites that can be hydrolyzed to 8-α-hydroxymutilin. The marker residue for tiamulin, according to Regulation EEC 2377/90, is the [...] Read more.
The administration of veterinary medicinal products containing tiamulin hydrogen fumarate (THF) leads to the appearance of the following residues in animal tissues: THF and metabolites that can be hydrolyzed to 8-α-hydroxymutilin. The marker residue for tiamulin, according to Regulation EEC 2377/90, is the sum of the metabolites that can be hydrolyzed to 8-α-hydroxymutilin. The main aim of this study was to analyze the depletion of tiamulin residues and metabolites that can be hydrolyzed to 8-α-hydroxymulinin by liquid chromatography with tandem mass spectrometry (LC-MS/MS) in pig, rabbit and bird tissues after tiamulin administration and to determine minimum withdrawal times for products of animal origin intended for human consumption. Tiamulin was administered orally as follows: 12,000 µg/kg body weight/day for 7 days to pigs and rabbits and 20,000 µg tiamulin/kg body weight/day for 7 days to broiler chickens and turkeys. The values found for tiamulin marker residues were 3 times higher in liver than in muscle in pigs, 6 times in rabbits and 8–10 times in birds. The content of tiamulin residues in eggs from laying hens was below 1000 µg/kg at all times of analysis. The minimum withdrawal times for animal products intended for human consumption, resulting from this study, are 5 days for pigs, rabbits and turkeys, 3 days for broiler chickens and 0 days for eggs. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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11 pages, 2356 KiB  
Article
Determination of Tyrosine Kinase Inhibitors via Capillary Electrophoresis with Tandem Mass Spectrometry and Online Stacking Preconcentration
by Jan Petr
Pharmaceuticals 2023, 16(2), 186; https://doi.org/10.3390/ph16020186 - 25 Jan 2023
Cited by 3 | Viewed by 1229
Abstract
Capillary electrophoresis connected with tandem mass spectrometry was employed for the development of a method for determination of various tyrosine kinase inhibitors in plasma samples. A stacking online preconcentration with a 120 cm-long capillary was used for the determination of bosutinib, dasatinib, canertinib, [...] Read more.
Capillary electrophoresis connected with tandem mass spectrometry was employed for the development of a method for determination of various tyrosine kinase inhibitors in plasma samples. A stacking online preconcentration with a 120 cm-long capillary was used for the determination of bosutinib, dasatinib, canertinib, and erlotinib at physiologically relevant concentrations. The optimization included both capillary electrophoresis and mass spectrometry steps. Under optimal conditions, 50 mM formic acid pH 2.5, an injection time of 120 s, and an optimized mass spectrometry set-up (as sheath liquid composition 75:24.9:0.1 (v/v) methanol, water, formic acid, and appropriate conditions for ion transitions), LODs in a range of 3.9–23.0 nmol·L−1 were observed. The method was validated in terms of linearity, limit of detection, limit of quantification, repeatability of migration times and peak area, and recovery using plasma as a matrix for analytes. The results showed that this method has great promise for use in many analytical tasks, e.g., therapeutic drug monitoring. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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25 pages, 5028 KiB  
Article
Development and Validation of an LC-MS/MS Method for the Quantitative Determination of Contezolid in Human Plasma and Cerebrospinal Fluid
by Guanxuanzi Zhang, Na Zhang, Liuhan Dong, Nan Bai and Yun Cai
Pharmaceuticals 2023, 16(1), 32; https://doi.org/10.3390/ph16010032 - 26 Dec 2022
Cited by 3 | Viewed by 1623
Abstract
To develop and verify a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determining contezolid in plasma and cerebrospinal fluid (CSF). Protein precipitation was performed on samples using linezolid as the internal standard. We used an Agilent EclipsePlus C18 column operating at 0.4 mL/min [...] Read more.
To develop and verify a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determining contezolid in plasma and cerebrospinal fluid (CSF). Protein precipitation was performed on samples using linezolid as the internal standard. We used an Agilent EclipsePlus C18 column operating at 0.4 mL/min in conjunction with acetonitrile and water mobile phases for the LC-MS/MS analysis. Using the precursor-product ion pairs 409.15→269.14 (contezolid) and 338.14→195.1 (linezolid), multiple reaction monitoring was used to quantify the compounds. Plasma linearity range was 50.0 to 5000 ng/mL, and CSF was 20.0 to 1000 ng/mL (r2 = 0.999). The inter-batch and intra-batch precisions were ≤2.57% and ≤5.79%, respectively. Plasma recovered 92.94%, and CSF recovered 97.83%. Plasma, CSF, hemolytic plasma, and hyperlipidemic plasma all showed a coefficient of variation ≤ 7.44%. The stability and dilution integrity of this method were also acceptable. The study also demonstrated that artificial CSF can be used as a matrix for the preparation of standard curve samples. A simple and accurate method was developed and validated for the determination of contezolid concentrations in human plasma and CSF, which may be useful for monitoring the therapeutic effect of central nervous system medications. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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16 pages, 3132 KiB  
Article
Insights into HPLC-MS/MS Analysis, Antioxidant and Cytotoxic Activity of Astragalus fruticosus against Different Types of Cancer Cell Lines
by Mohamed Fayez Dekinash, Tarek M. Okda, Ehab Kotb Elmahallawy, Fathy Kandil El-Fiky, Gamal Abd El Hay Omran, Emil Svajdlenka, Naief Dahran, Manal F. El-Khadragy, Wafa A. Al-Megrin and El Moataz Bellah Ali El Naggar
Pharmaceuticals 2022, 15(11), 1406; https://doi.org/10.3390/ph15111406 - 14 Nov 2022
Viewed by 1724
Abstract
Plants from the genus Astragalus are gaining attention for their pharmacological importance. However, the information available regarding the HPLC–MS/MS chemical profile of A. fruticosus is inadequate. In this study, we performed HPLC–MS/MS analysis using electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI). [...] Read more.
Plants from the genus Astragalus are gaining attention for their pharmacological importance. However, the information available regarding the HPLC–MS/MS chemical profile of A. fruticosus is inadequate. In this study, we performed HPLC–MS/MS analysis using electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI). We tentatively identified 11 compounds in the A. fruticosus methanolic extract, including five flavonoidal and six saponin glycosides. The extract showed moderate antioxidant activity with 21.05% reduction in DPPH UV absorption. The preliminary cytotoxic screening against seven human cancer cell lines using 100 μg/mL extract showed prominent cytotoxic potential against colorectal cancer HCT–116 with 3.368% cell viability. It also showed moderate cytotoxic potential against prostate (DU–145), ovarian (SKOV–3) and lung (A–549) cancer cell lines with cell viability of 14.25%, 16.02% and 27.24%, respectively. The IC50 of the total extract against HCT–116 and DU–145 cell lines were 7.81 μg/mL and 40.79 μg/mL, respectively. The observed cytotoxicity of the total methanolic extract from the leaves against colorectal cancer might facilitate future investigations on cytotoxic agent(s) for disease management. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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17 pages, 2185 KiB  
Article
Pelargonium sidoides Root Extract: Simultaneous HPLC Separation, Determination, and Validation of Selected Biomolecules and Evaluation of SARS-CoV-2 Inhibitory Activity
by Manal A. Alossaimi, May A. Alzeer, Fatma M. Abdel Bar and Mai H. ElNaggar
Pharmaceuticals 2022, 15(10), 1184; https://doi.org/10.3390/ph15101184 - 23 Sep 2022
Cited by 5 | Viewed by 3070
Abstract
This study aimed to establish a validated HPLC-UV analytical method for the determination of gallic acid, catechin, scopoletin, and umckalin in phytoformulations containing P. sidoides. Also, to assess the anti-SARS-CoV-2 effect of P. sidoides and these biomolecules in vitro. An HPLC-UV method [...] Read more.
This study aimed to establish a validated HPLC-UV analytical method for the determination of gallic acid, catechin, scopoletin, and umckalin in phytoformulations containing P. sidoides. Also, to assess the anti-SARS-CoV-2 effect of P. sidoides and these biomolecules in vitro. An HPLC-UV method was developed and verified by testing the commercial forms, Kalobin® and Umca®. It revealed low detectable scopoletin and high umckalin levels. Pelargonium sidoides exhibited a significant reduction of SARS-CoV-2-induced cytopathic effect in Vero E6 cells (IC50 13.79 μg/mL and selectivity index, SI 6.3), whereas scopoletin showed a remarkable anti-SARS-CoV-2 activity with better selectivity (IC50 17.79 μg/mL and SI 14.22). An in-silico prediction of the drugability indicated that the studied biomolecules are under the acceptable norms of Lipinski’s rule, water-soluble, and showed high GIT absorption and bioavailability. Docking study towards the essential molecular targets for viral replication and entry of SARS-CoV-2 indicated good binding affinity of scopoletin (−6.4 Kcal/mol) towards the interface region between the SARS-CoV-2 spike protein RBD and the ACE2 surface receptor indicating the probability of interference with the viral entry to the human cells and showed H-bonding with His-41 in the active site of the main protease which may explain its high antiviral activity. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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14 pages, 1943 KiB  
Article
In the Search for Novel, Isoflavone-Rich Functional Foods—Comparative Studies of Four Clover Species Sprouts and Their Chemopreventive Potential for Breast and Prostate Cancer
by Agnieszka Galanty, Monika Niepsuj, Marta Grudzińska, Paweł Zagrodzki, Irma Podolak and Paweł Paśko
Pharmaceuticals 2022, 15(7), 806; https://doi.org/10.3390/ph15070806 - 28 Jun 2022
Cited by 5 | Viewed by 2048
Abstract
Despite a significant amount of research, the relationship between a diet rich in isoflavones and breast and prostate cancer risk is still ambiguous. The purpose of the current study was to pre-select the potential candidate for functional foods among red, white, crimson, and [...] Read more.
Despite a significant amount of research, the relationship between a diet rich in isoflavones and breast and prostate cancer risk is still ambiguous. The purpose of the current study was to pre-select the potential candidate for functional foods among red, white, crimson, and Persian clover sprouts, cultured for different periods of time (up to 10 days), with respect to the isoflavone content (determined by HPLC-UV-VIS), and to verify their impact on hormone-dependent cancers in vitro. The red clover sprouts were the richest in isoflavones (up to 426.2 mg/100 g dw), whereas the lowest content was observed for the crimson clover. Each species produced isoflavones in different patterns, which refer to the germination time. Hormone-insensitive MDA-MB-231 breast cancer cells were more resistant to the tested extracts than estrogen-dependent MCF7 breast cancer cells. Regarding prostate cancer, androgen-dependent LNCap cells were most susceptible to the tested sprouts, followed by androgen-insensitive, high metastatic PC3, and low metastatic DU145 cells. The observed cytotoxic impact of the tested sprouts is not associated with isoflavone content, as confirmed by chemometric analysis. Furthermore, the sprouts tested revealed a high antioxidant potential, and were characterized by high safety for normal breast and prostate cells. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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23 pages, 2497 KiB  
Article
Flowers and Leaves Extracts of Stachys palustris L. Exhibit Stronger Anti-Proliferative, Antioxidant, Anti-Diabetic, and Anti-Obesity Potencies than Stems and Roots Due to More Phenolic Compounds as Revealed by UPLC-PDA-ESI-TQD-MS/MS
by Sabina Lachowicz-Wiśniewska, Anubhav Pratap-Singh, Ireneusz Kapusta, Angelika Kruszyńska, Andrzej Rapak, Ireneusz Ochmian, Tomasz Cebulak, Wioletta Żukiewicz-Sobczak and Paweł Rubiński
Pharmaceuticals 2022, 15(7), 785; https://doi.org/10.3390/ph15070785 - 23 Jun 2022
Cited by 7 | Viewed by 2240
Abstract
The present work aims to assess the biological potential of polyphenolic compounds in different parts (flowers, leaves, stems, and roots) of Stachys palustris L. Towards secondary metabolites profile, 89 polyphenolic compounds (PCs) were identified by UPLC-PDA-ESI-TQD-MS/MS, with a total average content of 6089 [...] Read more.
The present work aims to assess the biological potential of polyphenolic compounds in different parts (flowers, leaves, stems, and roots) of Stachys palustris L. Towards secondary metabolites profile, 89 polyphenolic compounds (PCs) were identified by UPLC-PDA-ESI-TQD-MS/MS, with a total average content of 6089 mg/100 g of dry matter (d.m.). In terms of biological activity, antioxidant activity (radical activity, reducing power), digestive enzyme inhibitory (α-glucosidase, α-amylase, pancreatic lipase) effect, and antiproliferative activity (inhibition of cell viability and induction of apoptosis in different human cancer cell lines) were explored. Leaves, flowers, stems, and roots of S. palustris L. have not been studied in this regard until now. Vescalagin and cocciferin d2, isoverbascoside (verbascoside), luteolin 6-C-glucoside, luteolin 6-C-galactoside, apigenin 6-C-glucoside, (−)-epicatechin, ellagic acid, and malvidin 3-O-diglucoside were detected as main ingredients in the studied parts. Methanolic extract of S. palustris L. leaves and flowers revealed the highest amount of PCs with the strongest antiradical (18.5 and 15.6 mmol Trolox equivalent (TE)/g d.m., respectively) and reducing power effects (7.3 and 5.6 mmol TE/g d.m.). Leaf extracts exhibited better α-amylase and pancreatic lipase inhibition effects, while flower extracts exhibited better α-glucosidase inhibition effect. Regarding antiproliferative activity, extracts of the leaves and flowers significantly reduced cell viability and induced a high level of apoptosis in human lung, pancreatic, bladder, and colon cancer cell lines, as well as in human acute myeloid leukemia; whereas the extracts from stems and roots revealed the weaker effects. The results of this work showed anti-proliferative and potentially anti-diabetic, anti-obesity properties of S. palustris L., especially for flowers and leaves, which may have wide potential applications in the functional food, special food, pharmaceutical, cosmetics industries, and/or in medicine. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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12 pages, 1765 KiB  
Article
Supercritical Fluid Chromatography—Tandem Mass Spectrometry for Rapid Quantification of Pentacyclic Triterpenoids in Plant Extracts
by Danil I. Falev, Denis V. Ovchinnikov, Ilya S. Voronov, Anna V. Faleva, Nikolay V. Ul’yanovskii and Dmitry S. Kosyakov
Pharmaceuticals 2022, 15(5), 629; https://doi.org/10.3390/ph15050629 - 20 May 2022
Cited by 7 | Viewed by 1963
Abstract
Pentacyclic triterpenoids (PCTs) are a widely distributed class of plant secondary metabolites. These compounds have high bioactive properties, primarily antitumor and antioxidant activity. In this study, a method was developed for the quantitative analysis of pentacyclic triterpenoids in plants using supercritical fluid chromatography–tandem [...] Read more.
Pentacyclic triterpenoids (PCTs) are a widely distributed class of plant secondary metabolites. These compounds have high bioactive properties, primarily antitumor and antioxidant activity. In this study, a method was developed for the quantitative analysis of pentacyclic triterpenoids in plants using supercritical fluid chromatography–tandem mass spectrometry (SFC-MS/MS). Separation of ten major PCTs (friedelin, lupeol, β-amyrin, α-amyrin, betulin, erythrodiol, uvaol, betulinic, oleanolic and ursolic acids) was studied on six silica-based reversed stationary phases. The best results (7 min analysis time in isocratic elution mode) were achieved on an HSS C18 SB stationary phase using carbon dioxide—isopropanol (8%) mobile phase providing decisive contribution of polar interactions to the retention of analytes. It was shown that the use of atmospheric pressure chemical ionization (APCI) is preferred over atmospheric pressure photoionization (APPI). The combination of SFC with APCI-MS/MS mass spectrometry made it possible to achieve the limits of quantification in plant extracts in the range of 2.3–20 μg·L−1. The developed method was validated and tested in the analyses of birch outer layer (Betula pendula) bark, and licorice (Glycyrrhiza glabra) root, as well as lingonberry (Vaccinium vitis-idaea), cranberry (Vaccinium oxycoccos), apple (Malus domestica “Golden Delicious” and Malus domestica “Red Delicious”) peels. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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27 pages, 3575 KiB  
Article
Application of Liquid Chromatography Coupled to Mass Spectrometry in Quality Assessment of Dietary Supplements—A Case Study of Tryptophan Supplements: Release Assay, Targeted and Untargeted Studies
by Krzysztof Adam Stępień and Joanna Giebułtowicz
Pharmaceuticals 2022, 15(4), 448; https://doi.org/10.3390/ph15040448 - 04 Apr 2022
Cited by 3 | Viewed by 2116
Abstract
Dietary supplements are widely consumed in the EU and the USA. Based on their similarity to pharmaceuticals, consumers mistakenly believe that dietary supplements have also been approved for safety and efficacy. However, in the absence of mandatory testing, data on supplement quality is [...] Read more.
Dietary supplements are widely consumed in the EU and the USA. Based on their similarity to pharmaceuticals, consumers mistakenly believe that dietary supplements have also been approved for safety and efficacy. However, in the absence of mandatory testing, data on supplement quality is scarce. Thus, we applied liquid chromatography coupled with tandem mass spectrometry to analyse the quality of dietary supplements containing tryptophan (Trp). We examined 22 supplements in tablets or capsules, produced in the USA, Great Britain, Germany, France, Czech Republic, and Poland. Trp release, crucial for bioavailability and efficiency, was assessed. Additionally, we performed a qualitative analysis of the main ingredient and screened for contaminants. Among the contaminants, we detected Trp’s metabolites, condensation products of Trp and carbonyl compounds, Trp degradation products, degradation products of kynurenine, and other contaminants such as glucosamine and melatonin. The main ingredient content was in the range of 55–100% in capsules and 69–87% in tablets. Surprisingly, almost no Trp release was noted from some supplements. Our study confirms the need to advance research on supplements. We believe that the high-quality analysis of supplements based on reliable analytical techniques will be an important contribution to the discussion on the regulatory framework of these products. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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11 pages, 664 KiB  
Article
UHPLC-MS/MS Analysis of Antibiotics Transfer and Concentrations in Porcine Oral Fluid after Intramuscular Application
by Anna Gajda, Ewelina Nowacka-Kozak, Małgorzata Gbylik-Sikorska and Piotr Cybulski
Pharmaceuticals 2022, 15(2), 225; https://doi.org/10.3390/ph15020225 - 14 Feb 2022
Cited by 3 | Viewed by 1796
Abstract
The monitoring of antibiotic use in animals is a crucial element to ensure food safety. The main goal of this study was to analyse the distribution of selected antibiotics to porcine oral fluid, as well as to demonstrate that an oral fluid is [...] Read more.
The monitoring of antibiotic use in animals is a crucial element to ensure food safety. The main goal of this study was to analyse the distribution of selected antibiotics to porcine oral fluid, as well as to demonstrate that an oral fluid is an alternative to other biological matrices used in the control of antibacterials. Therefore, an animal study with pigs treated using seven different antibiotics was performed. Sulfadoxine (SDX) with trimethoprim (TRMP), lincomycin (LIN), tiamulin (TIAM), tylosin (TYL), amoxicillin (AMX) and penicillin G (PEN G) were injected intramuscularly to pigs, and concentrations of these analytes in the oral fluid were assessed. Ultra-high-performance liquid chromatography coupled with mass spectrometry (UHPLC-MS/MS) was used to quantify the analytes. On the first day of medication, the highest concentrations for SDX and TRMP at the level of 22,300 µg/kg and 14,100 µg/kg were found, respectively. The concentrations of LIN (10,500 µg/kg) and TIAM (7600 µg/kg) were also relatively high. The peak of TYL was recorded on the second day of drug administration. Most of the analytes were present in oral fluid for 30 days, apart from TYL, which was detected for 27 days. It was found that AMX and PEN G were quantified only for 5 and 8 days, respectively, at very low concentrations. It was found that oral fluid can be used for the verification of antibiotics on pig farms. Full article
(This article belongs to the Special Issue Liquid Chromatography in Analysis of Bioactive Compounds for Pharmaceuticals, Cosmetics, and Functional Food Interest)
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