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Separations
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Current Trends in Chromatography for Bioanalytical Applications
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Current Trends in Chromatography for Bioanalytical Applications

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Bioanalysis/Clinical Analysis".

Deadline for manuscript submissions: closed (31 January 2022) | Viewed by 25488

Special Issue Editors

Prof. Dr. Irene Panderi

E-Mail Website
Guest Editor
Laboratory of Pharmaceutical Analysis, Division of Pharmaceutical Chemistry, School of Pharmacy, National and Kapodistrian University of Athens, Panepistimiopolis, Zografou, 15771 Athens, Greece
Interests: pharmaceutical analysis; analytical chemistry; analytical methods; drug analysis, metabolites; bioactive compounds; pharmaceuticals; cosmeceuticals
Special Issues, Collections and Topics in MDPI journals
Dr. Constantinos Pistos

E-Mail Website
Guest Editor
Department of Chemistry, West Chester University of Pennsylvania, West Chester, PA 19383, USA
Interests: forensic and clinical toxicological analysis; drug analysis; bioanalysis; instrumental analysis; method development and validation
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Chromatography is the most powerful analytical technique that allows for the separation of all the compounds in multicomponent chemical mixtures. Current trends in bioanalysis require the development of novel analytical procedures, including efficient sample collection and sample preparation protocols for the detection of compounds of interest at trace levels.

The target of this Special Issue is to present novel chromatographic methods using various sample collection and sample preparation techniques for the analysis of compounds of pharmaceutical interest with applications in bioanalysis, toxicology, doping control, medicine, and food chemistry.

With your rich expertise in the field of analytical chemistry, we believe that your contribution to this Special Issue will definitely have a significant impact on the entire scientific research community.

Prof. Dr. Irene Panderi
Assist. Prof. Dr. Constantinos Pistos
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. 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

  • drug analysis
  • bioanalysis
  • toxicology
  • doping control
  • food chemistry
  • medicine
  • dried blood spots

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Published Papers (5 papers)

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Research

15 pages, 11952 KiB  
Article
Development and Validation of a Novel HPLC Method for the Determination of Ephedrine Hydrochloride in Nasal Ointment
by Konstantinos Kallinteris, Kostas Gkountanas, Iοannis Karamitros, Haris Boutsikaris and Yannis Dotsikas
Separations 2022, 9(8), 198; https://doi.org/10.3390/separations9080198 - 1 Aug 2022
Cited by 9 | Viewed by 4467
Abstract
A simple, precise, and cost-effective reverse phase ion pair chromatographic (RP-IP-HPLC) method was developed and validated for the determination of Ephedrine Hydrochloride in a nasal ointment. A simple and fast extraction protocol was developed for the effective recovery of the analyte, and for [...] Read more.
A simple, precise, and cost-effective reverse phase ion pair chromatographic (RP-IP-HPLC) method was developed and validated for the determination of Ephedrine Hydrochloride in a nasal ointment. A simple and fast extraction protocol was developed for the effective recovery of the analyte, and for this purpose, Bromhexine Hydrochloride was used as the internal standard. The mobile phase consisted of MeOH, Sodium Lauryl Sulfate (SLS) 49.8 mM, triethylamine (ET3N) in the ratio of 65:34.6:0.4%, respectively, with pH = 2.20. The detection of the compounds was carried out at 206 nm, and we used a PDA detector. A short run time was achieved with retention times of 6.3 min and 9.8 min for ephedrine hydrochloride and the internal standard, respectively. The proposed method was validated according to ICH guidelines. Linearity was confirmed in the range of 50–150 μg/mL. Recoveries results were within the range of 98–102% and precision < 2% for the analyte in spiked blank matrix. Robustness testing was conducted via a fractional factorial experimental design. The method was found to fulfill the required specifications for specificity and stability for both standard solutions and samples, as well and applied to the determination of ephedrine hydrochloride in nasal ointments produced by the Greek Military Pharmaceutical Laboratories. Full article
(This article belongs to the Special Issue Current Trends in Chromatography for Bioanalytical Applications)
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13 pages, 635 KiB  
Article
A Validated RP-HPLC Method for the Determination of Butamirate Citrate and Benzoic Acid in Syrup, Based on an Experimental Design Assessment of Robustness
by Antonios-Dionysios G. Neofotistos, Kostas Gkountanas, Haris Boutsikaris and Yannis Dotsikas
Separations 2021, 8(10), 163; https://doi.org/10.3390/separations8100163 - 27 Sep 2021
Cited by 6 | Viewed by 5249
Abstract
A reversed-phase high-pressure liquid chromatography (RP-HPLC) method was developed and subsequently validated for the simultaneous determination of butamirate citrate (BC) and benzoic acid (BA) in cough syrup. The separation was performed employing a cyanopropyl column with a mobile phase consisting of 50%/50% v/v [...] Read more.
A reversed-phase high-pressure liquid chromatography (RP-HPLC) method was developed and subsequently validated for the simultaneous determination of butamirate citrate (BC) and benzoic acid (BA) in cough syrup. The separation was performed employing a cyanopropyl column with a mobile phase consisting of 50%/50% v/v MeOH/NaH2PO4 * H2O 50 mM aqueous solution pH = 3.0. The quantitation was achieved with a diode array detector (DAD) at 210 nm. The method demonstrated a congenitally satisfactory separation, yet the acquired peaks were asymmetrical. This effect was eliminated by using 1% triethylamine in the buffer solution as a silanol blocker. In addition, the method was found to unequivocally assess the target analytes in the sample matrix and fulfilled the required specifications in relevance to specificity, linearity, accuracy, precision and stability of both the standard solutions and of the sample solutions. Lastly, an experimental design was designed in order to assess the robustness of the proposed assay. To this purpose, a graphical and a statistical approach were utilized and compared to identify the factors that should be strictly controlled during each execution of the method. Full article
(This article belongs to the Special Issue Current Trends in Chromatography for Bioanalytical Applications)
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14 pages, 1471 KiB  
Article
Eco-Friendly UPLC-MS/MS Quantitation of Delafloxacin in Plasma and Its Application in a Pharmacokinetic Study in Rats
by Muzaffar Iqbal, Essam Ezzeldin, Md. Khalid Anwer and Faisal Imam
Separations 2021, 8(9), 146; https://doi.org/10.3390/separations8090146 - 6 Sep 2021
Cited by 10 | Viewed by 2874
Abstract
A novel UPLC-MS/MS assay was developed for rapid quantification of delafloxacin (a novel fluoroquinolone antibiotic in plasma samples by one step sample cleanup procedure. Delafloxacin (DFX) and internal standard (losartan) were separated on a UPLC BEH C18 column (50 × 2.1 mm; [...] Read more.
A novel UPLC-MS/MS assay was developed for rapid quantification of delafloxacin (a novel fluoroquinolone antibiotic in plasma samples by one step sample cleanup procedure. Delafloxacin (DFX) and internal standard (losartan) were separated on a UPLC BEH C18 column (50 × 2.1 mm; 1.7 μm) by using gradient programing of a mobile phase containing 0.1% formic acid in acetonitrile and 0.1% formic acid in water. The quantification was performed by a using triple-quadrupole mass detector at an electrospray ionization interface in positive mode. The precursor to the product ion transition of 441.1 → 379.1 for the qualifier and 441.1 → 423.1 for the quantifier was used for DFX monitoring, whereas 423.1 → 207.1 was used for the internal standard. The validation was performed as per guidelines of bioanalytical method validation, and the evaluated parameters were within the acceptable range. The greenness assessment of the method was evaluated by using AGREE software covering all 12 principles of green analytical chemistry. The final score obtained was 0.78, suggesting excellent greenness of the method. Moreover, Deming regression analysis showed an excellent linear relationship between this method and our previously reported method, and it is suitable for high-throughput analysis for routine application. The proposed method was effectively applied in a pharmacokinetic study of novel formulation (self-nanoemulsifying drug delivery systems) of DFX in rats. Full article
(This article belongs to the Special Issue Current Trends in Chromatography for Bioanalytical Applications)
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20 pages, 3348 KiB  
Article
Determination of 19 Psychoactive Substances in Premortem and Postmortem Whole Blood Samples Using Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry
by Sevasti Karampela, Jessica Smith and Irene Panderi
Separations 2021, 8(6), 78; https://doi.org/10.3390/separations8060078 - 3 Jun 2021
Cited by 6 | Viewed by 5864
Abstract
An ever-increasing need exists within the forensic laboratories to develop analytical processes for the qualitative and quantitative determination of a broad spectrum of new psychoactive substances. Phenylethylamine derivatives are among the major classes of psychoactive substances available on the global market and include [...] Read more.
An ever-increasing need exists within the forensic laboratories to develop analytical processes for the qualitative and quantitative determination of a broad spectrum of new psychoactive substances. Phenylethylamine derivatives are among the major classes of psychoactive substances available on the global market and include both amphetamine analogues and synthetic cathinones. In this work, an ultra-high-performance liquid chromatography-positive ion electrospray ionization tandem mass spectrometric method (UHPLC-ESI-MS/MS) has been developed and fully validated for the determination of 19 psychoactive substances, including nine amphetamine-type stimulants and 10 synthetic cathinone derivatives, in premortem and postmortem whole blood. The assay was based on the use of 1 mL premortem or postmortem whole blood, following solid phase extraction prior to the analysis. The separation was achieved on a Poroshell 120 EC-C18 analytical column with a gradient mobile phase of 0.1% formic acid in acetonitrile and 0.1% formic acid in water in 9 min. The dynamic multiple reaction monitoring used in this work allowed for limit of detection (LOD) and lower limit of quantitation (LOQ) values of 0.5 and 2 ng mL−1, respectively, for all analytes both in premortem and postmortem whole blood samples. A quadratic calibration model was used for the 12 quantitative analytes over the concentration range of 20–2000 ng mL−1, and the method was shown to be precise and accurate both in premortem and postmortem whole blood. The method was applied to the analysis of real cases and proved to be a valuable tool in forensic and clinical toxicology. Full article
(This article belongs to the Special Issue Current Trends in Chromatography for Bioanalytical Applications)
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Graphical abstract

13 pages, 1895 KiB  
Article
Determination of Trans-Anethole in Essential Oil, Methanolic Extract and Commercial Formulations of Foeniculum vulgare Mill Using a Green RP-HPTLC-Densitometry Method
by Ahmed I. Foudah, Faiyaz Shakeel, Mohammad H. Alqarni, Hasan. S. Yusufoglu, Mohammad A. Salkini and Prawez Alam
Separations 2020, 7(4), 51; https://doi.org/10.3390/separations7040051 - 29 Sep 2020
Cited by 8 | Viewed by 4889
Abstract
Due to the lack of ecofriendly/green reversed-phase high-performance thin-layer chromatography (RP-HPTLC) methods for trans-anethole (TAL) and its simplicity over routine analytical techniques, there was a necessity to establish a suitable HPTLC methodology for the quantitative analysis of TAL. Therefore, the first objective of [...] Read more.
Due to the lack of ecofriendly/green reversed-phase high-performance thin-layer chromatography (RP-HPTLC) methods for trans-anethole (TAL) and its simplicity over routine analytical techniques, there was a necessity to establish a suitable HPTLC methodology for the quantitative analysis of TAL. Therefore, the first objective of this research was to develop an accurate, rapid and green RP-HPTLC densitometry methodology for the quantitative analysis of TAL in essential oil, traditional and ultrasound-assisted extracts of Foeniculum vulgare Mill and commercial formulations. The second objective was to compare the traditional method of extraction of TAL with its ultrasound-assisted method of extraction. The chromatogram of TAL from essential oil and traditional and ultrasound-assisted extracts of fennel and commercial formulations was verified by recoding its single spectra at Rf = 0.31 ± 0.01 in comparison to standard TAL. The proposed analytical methodology has been found to be superior in terms of linearity, accuracy and precision compared to most of the reported analytical methods for TAL analysis. The amount of TAL in the essential oil of fennel was recorded as 8.82 mg per g of oil. The content of TAL in traditional extracts of fennel, formulation 1 (dietary supplement 1) and formulation 2 (dietary supplement 2), was recorded as 6.44, 4.88 and 4.48 mg per g, respectively. The amount of TAL in ultrasound-assisted extracts of fennel, formulation 1 and formulation 2, was recorded as 8.34, 6.46 and 5.81 mg per g, respectively. The ultrasound method of extraction of TAL was found to be better than the traditional method of extraction. The results of validation studies and phytochemical analysis showed that the proposed methodology could be efficiently utilized for the quantification of TAL in the wide range of products having TAL as a component. Full article
(This article belongs to the Special Issue Current Trends in Chromatography for Bioanalytical Applications)
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