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Analytica
Special Issues
New Analytical Techniques and Methods in Pharmaceutical Science
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New Analytical Techniques and Methods in Pharmaceutical Science

A special issue of Analytica (ISSN 2673-4532).

Deadline for manuscript submissions: 30 June 2025 | Viewed by 23290

Special Issue Editors

Prof. Dr. Dora Melucci

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Guest Editor
Department of Chemistry “Giacomo Ciamician”, Alma Mater Studiorum University of Bologna, Via Selmi 2, I-40126 Bologna, Italy
Interests: chemometrics; environmental chemistry; forensics; food chemistry; pharmaceutics
Special Issues, Collections and Topics in MDPI journals
Dr. Marcello Locatelli

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Guest Editor
Department of Pharmacy, University of G. d'Annunzio Chieti and Pescara, Chieti, Italy
Interests: innovative (micro) extraction procedures (MEPS, FPSE, DLLME, SULLE, MAE, etc.) and hyphenated instrument configurations; bioactive compounds (drugs, drugs associations, and natural bioactive compounds); characterization, fingerprints, and method validation; HPLC; mass spectrometry (MS and MS/MS)
Special Issues, Collections and Topics in MDPI journals
Dr. Angela Tartaglia

E-Mail Website
Guest Editor
Department of Pharmacy, University “G. d'Annunzio” of Chieti-Pescara, Via dei Vestini 31, 66100 Chieti, Italy
Interests: sample preparation; biological matrices; bioanalysis; microextraction procedures; separation techniques; chromatography
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Recently, increased demand for new formulations and new targeted therapies has led to more sensitive and selective analytical procedures for simultaneous classification, identification, and quantification of compounds that show different physical–chemical properties. These play a crucial role in pharmaceutical sciences and therapeutic drug monitoring and could provide identification and quantification data supporting drug discovery, drug synthesis, pharmacokinetic studies, drug–protein interactions, etc.

The present Special Issue will include review and full-length research articles focusing on analytical chemistry applied in drug design and drug action. Researchers working on method development and validation, separation methods in drug synthesis and purification, pharmacokinetics, drug delivery system, bioanalysis, drug toxicology research, etc. are cordially invited to contribute a research or review article in this Special Issue. The degree of novelty and the significance of the research will be scrutinized prior to the peer-reviewing process.

Prof. Dr. Dora Melucci
Prof. Dr. Marcello Locatelli
Dr. Angela Tartaglia
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. Analytica is an international peer-reviewed open access quarterly 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 1000 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 method
  • Therapeutic drug monitoring
  • Chemometric
  • Pharmaceutical applications
  • (micro)extraction procedures
  • Physical-chemical characterization
  • Drug development

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Published Papers (6 papers)

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Research

16 pages, 1071 KiB  
Article
Determination of the Active Pharmaceutical Ingredients in Saridon Tablets Using an Economical and Sensitive Thin Layer Chromatography Method Combined with Densitometry
by Alina Pyka-Pająk
Analytica 2024, 5(1), 1-16; https://doi.org/10.3390/analytica5010001 - 2 Jan 2024
Viewed by 2385
Abstract
A new TLC–densitometric method has been developed for the identification and quantification of paracetamol (PA), propyphenazone (PP) and caffeine (C) in Saridon tablets using the NP-TLC technique combined with densitometry. This method allows for the simultaneous determination of PA, PP, and C in [...] Read more.
A new TLC–densitometric method has been developed for the identification and quantification of paracetamol (PA), propyphenazone (PP) and caffeine (C) in Saridon tablets using the NP-TLC technique combined with densitometry. This method allows for the simultaneous determination of PA, PP, and C in the same sample. Among all the tested chromatographic conditions, the mixture consisting of chloroform + toluene + ethyl acetate + ethanol + acetic acid (18:18:7.5:5.0:0.3, v/v/v/v/v) and a silica gel 60F254 plate proved to be the most effective for the separation of the three tested active pharmaceutical ingredients (APIs) and substances related to paracetamol. The full validation of the proposed NP-TLC method proved that it is specific, precise, accurate, robust and sensitive. The percentage content in relation to the content declared by the manufacturer was for propyphenazone 99.8%, paracetamol 101.6% and caffeine 100.8%, which was in accordance with pharmacopoeial requirements. The results presented indicate the possibility of using the developed method in the routine control of pharmaceutical preparations containing these APIs. The proposed method is economical and more sensitive compared to the previously proposed planar methods for the simultaneous determination of APIs. What is more, the presented method may be an excellent economical alternative when the HPLC method is unavailable for such a determination. Full article
(This article belongs to the Special Issue New Analytical Techniques and Methods in Pharmaceutical Science)
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14 pages, 3650 KiB  
Article
Compatibility Study between Fenbendazole and Polymeric Excipients Used in Pharmaceutical Dosage Forms Using Thermal and Non-Thermal Analytical Techniques
by Gilberto S. N. Bezerra, Vicente F. Moritz, Tielidy A. de M. de Lima, Declan M. Colbert, Joseph Geever and Luke Geever
Analytica 2022, 3(4), 448-461; https://doi.org/10.3390/analytica3040031 - 12 Dec 2022
Cited by 4 | Viewed by 3868
Abstract
The body of work described in this research paper evaluates the compatibility between Fenbendazole (Fen), which is a broad-spectrum anthelmintic with promising antitumor activity, and three polymeric excipients commonly applied in pharmaceutical dosage forms. The assessment of binary mixtures was performed by differential [...] Read more.
The body of work described in this research paper evaluates the compatibility between Fenbendazole (Fen), which is a broad-spectrum anthelmintic with promising antitumor activity, and three polymeric excipients commonly applied in pharmaceutical dosage forms. The assessment of binary mixtures was performed by differential scanning calorimetry and thermogravimetric analysis/derivative thermogravimetry to predict physical and/or chemical interactions, followed by X-ray diffraction spectroscopy (XRD), Fourier transform infrared spectroscopy (FTIR), and high-performance liquid chromatography (HPLC) to confirm or exclude any interactions. Thermal studies suggested the presence of interactions between Fen and P 407, PCL, and PLA. To validate these data, XRD showed that Fen is compatible with PCL and PLA, suggesting some interaction with P 407. FTIR demonstrated that PCL and PLA can establish physical interactions with Fen; moreover, it suggested that P 407 interacts not only physically but also chemically, which was later proved by HPLC to be only new intermolecular interactions. This work supports the further application of P 407, PCL, and PLA for the development of new medicinal and veterinary formulations containing Fen, since they do not affect the physical and chemical characteristics of the active ingredient and consequently its bioavailability and therapeutic efficacy. Full article
(This article belongs to the Special Issue New Analytical Techniques and Methods in Pharmaceutical Science)
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12 pages, 1761 KiB  
Communication
General Applicability of High-Resolution Continuum-Source Graphite Furnace Molecular Absorption Spectrometry to the Quantification of Oligopeptides Using the Example of Glutathione
by Daniel Baecker and Sebastian Guenther
Analytica 2022, 3(1), 24-35; https://doi.org/10.3390/analytica3010003 - 16 Jan 2022
Cited by 4 | Viewed by 3447
Abstract
This communication introduces the first-time application of high-resolution continuum-source molecular absorption spectrometry (HR CS MAS) for the quantification of a peptide. The graphite furnace technique was employed and the tripeptide glutathione (GSH) served as a model compound. Based on measuring sulfur in terms [...] Read more.
This communication introduces the first-time application of high-resolution continuum-source molecular absorption spectrometry (HR CS MAS) for the quantification of a peptide. The graphite furnace technique was employed and the tripeptide glutathione (GSH) served as a model compound. Based on measuring sulfur in terms of carbon monosulfide (CS), a method was elaborated to analyze aqueous solutions of GSH. The most prominent wavelength of the CS molecule occurred at 258.0560 nm and was adduced for monitoring. The methodological development covered the optimization of the pyrolysis and vaporization temperatures. These were found optimally to be 250 °C and 2250 °C, respectively. Moreover, the effect of modifiers (zirconium, calcium, magnesium, palladium) on the absorption signals was investigated. The best results were obtained after permanent coating of the graphite tube with zirconium (total amount of 400 μg) and adding a combination of palladium (10 µL, 10 g L−1) and calcium (2 µL, 1 g L−1) as a chemical modifier to the probes (10 µL). Aqueous standard samples of GSH were used for the calibration. It showed a linear range of 2.5–100 µg mL−1 sulfur contained in GSH with a correlation coefficient R2 > 0.997. The developed method exhibited a limit of detection (LOD) and quantification (LOQ) of 2.1 µg mL−1 and 4.3 µg mL−1 sulfur, respectively. The characteristic mass accounted for 5.9 ng sulfur. The method confirmed the general suitability of MAS for the analysis of an oligopeptide. Thus, this study serves as groundwork for further development in order to extend the application of classical atomic absorption spectrometry (AAS). Full article
(This article belongs to the Special Issue New Analytical Techniques and Methods in Pharmaceutical Science)
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9 pages, 1824 KiB  
Article
Hydrophilic Interaction Liquid Chromatography Coupled with Fluorescence Detection (HILIC-FL) for the Quantitation of Octreotide in Injection Forms
by Eleni Doulou, Marina Kalomiraki, Anthi Parla, Kyriaki Thermos, Nikos A. Chaniotakis and Irene Panderi
Analytica 2021, 2(4), 121-129; https://doi.org/10.3390/analytica2040012 - 1 Oct 2021
Cited by 6 | Viewed by 3721
Abstract
Octreotide is a synthetic cyclic octapeptide analogue of somatostatin-14. It is mainly administered for the treatment of acromegaly, severe diarrhea, and neuroendocrine neoplasias. In this work, a hydrophilic interaction liquid chromatography (HILIC) method with fluorescence (FL) detection was developed and validated for the [...] Read more.
Octreotide is a synthetic cyclic octapeptide analogue of somatostatin-14. It is mainly administered for the treatment of acromegaly, severe diarrhea, and neuroendocrine neoplasias. In this work, a hydrophilic interaction liquid chromatography (HILIC) method with fluorescence (FL) detection was developed and validated for the quantitation of octreotide in solutions for injection. Chromatographic separation was performed on an XBridge®-HILIC analytical column under isocratic elution with a short chromatographic run time of less than 10 min. The mobile phase consisted of ammonium bicarbonate 8.6 mM (pH 8.1)/acetonitrile 35/65 (v/v). The high sensitivity and selectivity of the fluorescence detection, with the excitation wavelength (λexcitation) set at 280 nm and the emission wavelength set at (λemission) 330 nm, enabled a simple sample preparation procedure that included only dilution steps. The calibration curve showed good linearity with a correlation coefficient greater than 0.998. The method was successfully applied to the analysis of commercially available octreotide injection forms. Full article
(This article belongs to the Special Issue New Analytical Techniques and Methods in Pharmaceutical Science)
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9 pages, 1789 KiB  
Article
An Authentication Study on Grappa Spirit: The Use of Chemometrics to Detect a Food Fraud
by Silvia Arduini, Alessandro Zappi, Marcello Locatelli, Salvatore Sgrò and Dora Melucci
Analytica 2021, 2(3), 84-92; https://doi.org/10.3390/analytica2030010 - 30 Aug 2021
Cited by 1 | Viewed by 3621
Abstract
An authenticity study on Italian grape marc spirit was carried out by gas chromatography (GC) and chemometrics. A grape marc spirit produced in Italy takes the particular name of “grappa”, a product which has peculiar tradition and production in its country [...] Read more.
An authenticity study on Italian grape marc spirit was carried out by gas chromatography (GC) and chemometrics. A grape marc spirit produced in Italy takes the particular name of “grappa”, a product which has peculiar tradition and production in its country of origin. Therefore, the evaluation of its authenticity plays an important role for its consumption in Italy, as well as for its exportation all around the world. For the present work, 123 samples of grappa and several kinds of spirits were analyzed in their alcohol content by electronic densimetry, and in their volatile fraction by gas-chromatography with a flame-ionization detector. Part of these samples (94) was employed as a training set to compute a chemometric model (by linear discriminant analysis, LDA) and the other part (29 samples) was used as a test set to validate it. Finally, two grappa samples seized from the market by the Italian Customs and Monopolies Agency and considered suspicious due to their aroma reported as non-compliant were projected onto the LDA model to evaluate the compliance with the “grappa” class. A further one-class classification method by principal component analysis (PCA) was carried out to evaluate the compliance with other classes. Results showed that the suspicious samples were not recognized as belonging to any of the analyzed spirit classes, confirming the starting hypothesis that they could be grappa samples adulterated in some way. Full article
(This article belongs to the Special Issue New Analytical Techniques and Methods in Pharmaceutical Science)
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8 pages, 626 KiB  
Article
Thallium: A Polluting Metal of New Generation. Its Voltammetric Determination in Herbal Medicines in Presence of Metal Interferences
by Dora Melucci, Sonia Casolari, Marcello Locatelli and Clinio Locatelli
Analytica 2021, 2(3), 76-83; https://doi.org/10.3390/analytica2030009 - 3 Aug 2021
Cited by 2 | Viewed by 3294
Abstract
The present paper reports a new application: the voltammetric determination in herbal medicines of ultra-trace thallium(I), in the presence of lead(II), tin(II) and antimony(III) as interfering metals, by square wave anodic stripping voltammetry (SWASV). A conventional three-electrodes voltammetric cell was employed with a [...] Read more.
The present paper reports a new application: the voltammetric determination in herbal medicines of ultra-trace thallium(I), in the presence of lead(II), tin(II) and antimony(III) as interfering metals, by square wave anodic stripping voltammetry (SWASV). A conventional three-electrodes voltammetric cell was employed with a stationary hanging mercury drop electrode (HMDE) as working electrode and a platinum electrode and an Ag|AgCl|KClsatd. electrode as auxiliary and reference electrodes, respectively. The supporting electrolyte was 0.5 mol L−1 ammonium citrate buffer pH 6.5 + 7.3·10−3 mol L−1 EDTA-Na2. The analytical procedure was verified by the analysis of the standard reference materials: spinach Leaves NIST-SRM 1570a and tomato leaves NIST-SRM 1573a from National Institute of Standards and Technology. Precision and trueness, expressed as relative standard deviation and relative error, respectively, were generally lower than 7% in all cases. Once set up on the standard reference materials, the analytical procedure was transferred and applied to herbal medicines samples—Taraxacun officinale weber, Eucalyptus globulus and Harpagophytum procumbens DC—sold on the market. A critical comparison with spectroscopic measurements is also discussed. Full article
(This article belongs to the Special Issue New Analytical Techniques and Methods in Pharmaceutical Science)
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