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Separations
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Innovation of Analysis Methods in Pharmaceutical Chemistry
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Innovation of Analysis Methods in Pharmaceutical Chemistry

A special issue of Separations (ISSN 2297-8739).

Deadline for manuscript submissions: closed (20 February 2022) | Viewed by 14871

Special Issue Editor

Dr. Giorgio Marrubini

E-Mail Website1 Website2
Guest Editor
Department of Drug Sciences, University of Pavia, Pavia, Italy
Interests: analytical chemistry; pharmaceutical analysis; analytical toxicology; method validation; robustness testing; chromatographic techniques; data analysis; design of experiments (DoE)
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Compendial and other official chromatographic methods often give the impression of being awkward and/or old-fashioned. This is mainly because chromatography base materials, and the chemical modifications thereof as well as the instruments, have been continuously improved over the years, but where the methods have not kept up with speed and performance. In pharmaceutical analysis, this subject is of particular relevance. It is a general feeling that there is the need to modernize many of the existing monographs both in terms of the materials that can be used and to find alternative separation mode solutions. HPLC columns of traditional format (250x4.6 mm, packed with particles of 10 or 5 microns diameter) are obsolete and could be successfully replaced by greener and more efficient columns having smaller formats. Also, modern materials for stationary phases do not suffer any more of the problems of the past, such as metals contamination and free silanols secondary interactions. Therefore, a change in the composition of the mobile phase may also be necessary when it comes to the time to change the old column used for a compendial method.

Ion-chromatography and Hydrophilic Interaction Liquid Chromatography (HILIC) have been shown as valuable complements to reversed-phase LC and are today viable and robust options together with normal-phase LC.

As strong evidence of this trend, the United States Pharmacopoeia (USP), for about ten years, started a global initiative to modernize existing monographs actively seeking industry collaborators to assist in the development of new monographs. Also, the scientific community is expecting soon the release of the final document of ICH Q14 “Analytical Procedure Development and Revision of Q2(R1) Analytical Validation” guideline that should list new requirements for validation of measurement methods.

This Special Issue aims to present readers with the latest research regarding method scaling, alternative separation mode solutions, and innovative approaches to tackle pharmaceutical analysis. The issue invites contributions relating, but not limited to, innovation in chromatographic pharmaceutical analysis, method development, and multivariate tools for data treatment.

Dr. Giorgio Marrubini
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

  • phamaceutical analysis
  • USP alternative methods
  • method scaling
  • method adaptations
  • ion chromatography
  • HILIC
  • multivariate approaches
  • design of Experiments
  • quality by Design
  • changes in compendial methods

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Published Papers (4 papers)

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Research

13 pages, 823 KiB  
Communication
Expanding Antineoplastic Drugs Surface Monitoring Profiles: Enhancing of Zwitterionic Hydrophilic Interaction Methods
by Stefano Dugheri, Nicola Mucci, Donato Squillaci, Elisabetta Bucaletti, Giovanni Cappelli, Lucia Trevisani, Cecile Valsecchi, Viviana Consonni, Fabio Gosetti, Davide Ballabio and Giulio Arcangeli
Separations 2022, 9(2), 34; https://doi.org/10.3390/separations9020034 - 29 Jan 2022
Cited by 2 | Viewed by 2794
Abstract
Antineoplastic drugs are a wide and heterogeneous group of substances that, as universally known, can cause highly severe toxic effects to whoever is exposed. From an occupational safety point of view, surface contaminations inside preparation and administration units are a growing issue and [...] Read more.
Antineoplastic drugs are a wide and heterogeneous group of substances that, as universally known, can cause highly severe toxic effects to whoever is exposed. From an occupational safety point of view, surface contaminations inside preparation and administration units are a growing issue and therefore require the development and implementation of sensible and fast monitoring methods. The unlikelihood of a unique all-embracing chromatography, able to correctly retain and separate each analyte led to the need to create an orthogonal normal phase analysis, which might be able to fill the gaps in the more common reversed-phase ones. An existing hydrophilic interaction method has thus been expanded to 6 other drugs and applied to real samples after an evaluation of its performances. The experimental data were then used to evaluate the possibility of estimating reliable relationships between the chromatographic retention and the chemical-structural features of the drugs under analysis. Full article
(This article belongs to the Special Issue Innovation of Analysis Methods in Pharmaceutical Chemistry)
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16 pages, 2257 KiB  
Article
Validated Modernized Assay for Foscarnet in Pharmaceutical Formulations Using Suppressed Ion Chromatography Developed through a Quality by Design Approach
by Ngoc Phuoc Dinh, Adel Shamshir, Gjani Hulaj and Tobias Jonsson
Separations 2021, 8(11), 209; https://doi.org/10.3390/separations8110209 - 5 Nov 2021
Cited by 3 | Viewed by 3479
Abstract
Inspired by the United States Pharmacopoeia (USP) “monograph modernization” initiative, we developed and validated an assay for foscarnet sodium injection solution (“foscavir”), following quality by design (QbD) principles, incorporating design of experiments (DoE) and multivariate data analysis to establish the design space and [...] Read more.
Inspired by the United States Pharmacopoeia (USP) “monograph modernization” initiative, we developed and validated an assay for foscarnet sodium injection solution (“foscavir”), following quality by design (QbD) principles, incorporating design of experiments (DoE) and multivariate data analysis to establish the design space and robust setpoint of the method. The resulting analytical procedure was based on ion chromatography (IC) with suppressed conductivity detection, employing an isocratic carbonate–bicarbonate eluent system. The assay was successfully validated at the robust setpoint conditions, according to the guidelines established by the International Council for Harmonization (ICH). The linear range stretched at least from 5 to 100 mg/L with high repeatability (relative standard deviation, RSD ≤ 0.3%) both at the target concentration (60 mg/L) and at 50% and 150% from this level. Special attention was given to establish a rugged assay that would be easily transferable between laboratories, and the recorded recoveries of 98.2–100.5% for both the formulated drug product and the drug substance during intermediate precision evaluation at different analysis situations indicated that this mission was accomplished. A multivariate assessment of intermediate precision data acquired using an experimental design scheme revealed that the assay was not adversely affected by any of the situation variables, including the use of different liquid chromatography instrument types, regardless of if they were constructed from inert materials or stainless steel that had been passivated, even though such problems have been reported in several previous methods for analysis of foscarnet. Full article
(This article belongs to the Special Issue Innovation of Analysis Methods in Pharmaceutical Chemistry)
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14 pages, 19629 KiB  
Article
Rhamnolipid Biosurfactants—Possible Natural Anticancer Agents and Autophagy Inhibitors
by Severina Semkova, Georgi Antov, Ivan Iliev, Iana Tsoneva, Pavel Lefterov, Nelly Christova, Lilyana Nacheva, Ivanka Stoineva, Lyudmila Kabaivanova, Galya Staneva and Biliana Nikolova
Separations 2021, 8(7), 92; https://doi.org/10.3390/separations8070092 - 28 Jun 2021
Cited by 17 | Viewed by 3552
Abstract
Background/Aim: A number of biologically active substances were proved as an alternative to conventional anticancer medicines. The aim of the study is in vitro investigation of the anticancer activity of mono- and di-Rhamnolipids (RL-1 and RL-2) against human breast cancer. Additionally, the combination [...] Read more.
Background/Aim: A number of biologically active substances were proved as an alternative to conventional anticancer medicines. The aim of the study is in vitro investigation of the anticancer activity of mono- and di-Rhamnolipids (RL-1 and RL-2) against human breast cancer. Additionally, the combination with Cisplatin was analyzed. Materials and Methods: Breast cell lines (MCF-10A, MCF-7 and MDA-MB-231) were treated with RLs and in combination with Cisplatin. The viability was analyzed using MTT assay, and investigation of autophagy was performed via acridine orange staining. Results: In contrast to the healthy cells, both tested cancer lines exhibited sensitivity to RLs treatment. This effect was accompanied by an influence on the autophagy-related acidic formation process. Only for the triple-negative breast cancer cell line (MDA-MB-231) the synergistic effect of the combined treatment (10 µM Cisplatin and 1 µg/mL RL-2) was observed. Conclusion: Based on studies on the reorganization of membrane models in the presence of RL and the data about a higher amount of lipid rafts in cancer cell membranes than in non-tumorigenic, we suggest a possible mechanism of membrane remodelling by formation of endosomes. Shortly, in order to have a synergistic effect, it is necessary to have Cisplatin andRL-2 as RL2 is a molecule inducingpositive membrane curvature. Full article
(This article belongs to the Special Issue Innovation of Analysis Methods in Pharmaceutical Chemistry)
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15 pages, 665 KiB  
Article
Characterization and Separation of Platinum-Based Antineoplastic Drugs by Zwitterionic Hydrophilic Interaction Liquid Chromatography (HILIC)–Tandem Mass Spectrometry, and Its Application in Surface Wipe Sampling
by Stefano Dugheri, Nicola Mucci, Enrico Mini, Donato Squillaci, Giorgio Marrubini, Gianluca Bartolucci, Elisabetta Bucaletti, Giovanni Cappelli, Lucia Trevisani and Giulio Arcangeli
Separations 2021, 8(5), 69; https://doi.org/10.3390/separations8050069 - 20 May 2021
Cited by 4 | Viewed by 3852
Abstract
Platinum-based antineoplastic drugs (PtADs) are among the most important and used families of chemotherapy drugs, which, even showing severe side effects and being hindered by drug resistance, are not likely to be replaced clinically any time soon. The growing interest in the occupational [...] Read more.
Platinum-based antineoplastic drugs (PtADs) are among the most important and used families of chemotherapy drugs, which, even showing severe side effects and being hindered by drug resistance, are not likely to be replaced clinically any time soon. The growing interest in the occupational health community in antineoplastic drug (AD) surface contamination requires the development of increasingly fast and easy high-throughput monitoring methods, even considering the lack of harmonized legally binding regulation criteria. Thus, a wipe sampling method together with zwitterionic hydrophilic interaction liquid chromatography (HILIC-Z)–tandem mass spectrometry (MS/MS) analysis was developed for the simultaneous evaluation of oxaliplatin, cisplatin, and carboplatin surface contaminations. A design of experiments approach was used to optimize the chromatographic conditions. Limits of quantification ranging from 2 to 5 ng/mL were obtained from interday and intraday repetitions for oxaliplatin and carboplatin, and between 170 and 240 ng/mL for cisplatin. The wipe desorption procedure is equivalent to other AD sampling methods, enabling a fast sample preparation, with an LC-MS/MS analysis time of less than 7 min. Full article
(This article belongs to the Special Issue Innovation of Analysis Methods in Pharmaceutical Chemistry)
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