Search for Articles:
Title / Keyword
Author / Affiliation / Email
Journal
Article Type
 
 
Advanced Search
 
Section
Special Issue
Volume
Issue
Number
Page
 
3.0
2.5
Journals
Separations
Special Issues
Application of Liquid Chromatography in Pharmaceutical and Toxicological Analysis
share announcement

Application of Liquid Chromatography in Pharmaceutical and Toxicological Analysis

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Chromatographic Separations".

Deadline for manuscript submissions: closed (20 October 2024) | Viewed by 9889

Special Issue Editors

Dr. Maria Nieddu

E-Mail Website
Guest Editor
Department of Medicine, Surgery and Pharmacy, University of Sassari, 07100 Sassari, Italy
Interests: liquid chromatography; mass spectrometry detection; UV-detection; sample preparation; method validation; pharmaceutical analysis; forensic analysis; biological matrices; extraction methods
Dr. Elena Baralla

E-Mail Website
Guest Editor
Department of Veterinary Medicine, University of Sassari, 07100 Sassari, Italy
Interests: toxicology; animal matrices; antioxidants
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

We are pleased to invite you to publish in this Special Issue focused on the application of liquid chromatography in pharmaceutical and toxicological analysis.

In pharmaceutical and toxicological fields, chromatography is one of the most used analytical methods for the identification and quantification of xenobiotics and their metabolites.

Different chromatographic techniques have been developed for the qualitative-quantitative determination of drugs according to their characteristics. Among these techniques, in particular, High-Performance Liquid Chromatography (HPLC) is the most used for pharmaceutical and toxicological purposes. The success of liquid chromatography in the development of rapid and precise analytical methods is that it provides good specificity and sensitivity. Sample pretreatment is an important factor to be considered to provide a selective chromatographic analysis. The use of specific purification techniques provides a sample that is relatively free of interferences, compatible with the analytical method, and that does not damage instrumentation. It is further desirable to concentrate the analytes for improved detection.

This Special Issue aims to provide an overview of applications of liquid chromatography in pharmaceutical and toxicological analysis, including both human and veterinary medicine.

In this Special Issue, original research articles and reviews as well as short communications are welcome. Research areas may include (but are not limited to) the following: liquid chromatography applied to analytical methods for drugs determination in biological matrices or pharmaceutical formulations, forensic and toxicological analysis, residue analysis, sample preparation, and development and validation of new analytical methods.

We look forward to receiving your contributions.

Dr. Maria Nieddu
Dr. Elena Baralla
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

  • liquid chromatography
  • drug analysis
  • forensic analysis
  • toxicological analysis
  • residues analysis
  • sample preparation
  • method validation
  • biological matrices
  • pharmaceutical preparation

Benefits of Publishing in a Special Issue

  • Ease of navigation: Grouping papers by topic helps scholars navigate broad scope journals more efficiently.
  • Greater discoverability: Special Issues support the reach and impact of scientific research. Articles in Special Issues are more discoverable and cited more frequently.
  • Expansion of research network: Special Issues facilitate connections among authors, fostering scientific collaborations.
  • External promotion: Articles in Special Issues are often promoted through the journal's social media, increasing their visibility.
  • e-Book format: Special Issues with more than 10 articles can be published as dedicated e-books, ensuring wide and rapid dissemination.

Further information on MDPI's Special Issue polices can be found here.

Published Papers (5 papers)

Download All Papers
Order results
Result details
Show export options expand_more Show export options expand_less
Select all
Export citation of selected articles as:

Research

Jump to: Review

14 pages, 1625 KiB  
Article
The Development and Validation of an LC–Orbitrap–HRMS Method for the Analysis of Four Tetracyclines in Milk and Its Application to Determine Oxytetracycline Concentrations after Intramuscular Administration in Healthy Sarda Ewes and Those Naturally Infected with Streptococcus uberis
by Severyn Salis, Simone Dore, Nicola Rubattu, Vittoria D’Ascenzo, Francesca T. Cherchi and Stefano A. Lollai
Separations 2024, 11(8), 242; https://doi.org/10.3390/separations11080242 - 8 Aug 2024
Viewed by 861
Abstract
An LC–Orbitrap–HRMS method was developed and validated for the simultaneous determination of four tetracyclines—oxytetracycline (OTC), tetracycline (TC), doxycycline (DC), and chlortetracycline (CTC)—in milk. This method involves sample extraction with McIlvaine–EDTA buffer solution (pH 4) and solid-phase extraction (SPE) with Oasis HLB cartridges, followed [...] Read more.
An LC–Orbitrap–HRMS method was developed and validated for the simultaneous determination of four tetracyclines—oxytetracycline (OTC), tetracycline (TC), doxycycline (DC), and chlortetracycline (CTC)—in milk. This method involves sample extraction with McIlvaine–EDTA buffer solution (pH 4) and solid-phase extraction (SPE) with Oasis HLB cartridges, followed by the evaporation of the extract and its reconstitution with a 14% methanol aqueous solution before injection into the instrumental system. This method has been validated in terms of linearity, sensitivity, selectivity, precision, and accuracy, in accordance with Commission Decision 2002/657/EC requirements. Compared to existing methods, this approach optimally combines a quantitative procedure for extracting analytes from the milk of different species, including sheep, bovines, and goats, with a very short LC–Orbitrap–HRMS instrumental analysis time (only 8 min), simultaneously ensuring high precision, sensitivity, and applicability as a rapid confirmation method in official food control laboratories. The proposed method was applied to determine the concentration levels of OTC in milk samples derived from healthy Sardinian sheep and those naturally infected with Streptococcus uberis, after the intramuscular administration of an antibiotic, in order to evaluate how much of the drug was “subtracted” during penetration from blood into milk, with a potential effect of reducing its therapeutic efficacy. Full article
(This article belongs to the Special Issue Application of Liquid Chromatography in Pharmaceutical and Toxicological Analysis)
►▼ Show Figures

Figure 1

11 pages, 1578 KiB  
Article
Improving the Current European Pharmacopoeia Enantio-Selective HPLC Method for the Determination of Enantiomeric Purity in Atorvastatin Calcium Salt Drug Substance
by Francesca Romana Mammone, Daniele Sadutto, Giulia D’Ettorre, Antonina Mosca and Roberto Cirilli
Separations 2024, 11(5), 154; https://doi.org/10.3390/separations11050154 - 16 May 2024
Viewed by 1311
Abstract
Atorvastatin (ATV) is a well-established lipid-lowering agent. ATV has two stereogenic centers, and of the four possible stereoisomers, only the (3R,5R) form is used therapeutically. The European Pharmacopoeia (EP) monograph 2022 for ATV calcium salt describes a normal-phase high-performance [...] Read more.
Atorvastatin (ATV) is a well-established lipid-lowering agent. ATV has two stereogenic centers, and of the four possible stereoisomers, only the (3R,5R) form is used therapeutically. The European Pharmacopoeia (EP) monograph 2022 for ATV calcium salt describes a normal-phase high-performance liquid chromatography (HPLC) method for the determination of enantiomeric purity in both drug substance and working standard samples, based on a 150 mm × 4.6 mm Chiralpak AD-H column. The main problems with this method are the very long analysis time and the high solvent consumption. Here, an alternative chromatographic protocol was developed using the Chiralpak AD-3 column (250 mm × 4.6 mm) packed with 3 μm silica particles instead of the 5 μm silica particles of the Chiralpak AD-H chiral stationary phase and characterized by the same polysaccharide selector, amylose-tris(3,5-dimethylphenylcarbamate). Using a mobile phase consisting of a mixture of n-hexane-ethanol-formic acid 90:10:0.1 (v/v/v) as the mobile phase and setting the flow rate and column temperature to 1.0 mL min−1 and 35 °C, respectively, a simultaneous stereo-selective separation was achieved within 35 min without observing any overlap between the enantiomeric impurity peak and peaks related to other ATV impurities. Compared to HPLC EP conditions, the analysis time to elute all the potentially related substances was faster and significantly less mobile phase volume was required. The linearity of the method has been demonstrated in the range of 4.4 μg mL−1 to 1000 μg mL−1 (R2 > 0.999). At a concentration of 4.4 μg mL−1, which is 0.075% of the test solution (5.8 mg mL−1, as ATV free acid), the signal-to-noise ratio was found to be 20. Full article
(This article belongs to the Special Issue Application of Liquid Chromatography in Pharmaceutical and Toxicological Analysis)
►▼ Show Figures

Figure 1

13 pages, 1787 KiB  
Article
An LC–MS/MS Analytical Method for Quantifying Tepotinib in Human Liver Microsomes: Application to In Vitro and In Silico Metabolic Stability Estimation
by Mohamed W. Attwa, Gamal A. E. Mostafa, Haitham AlRabiah and Adnan A. Kadi
Separations 2023, 10(6), 330; https://doi.org/10.3390/separations10060330 - 26 May 2023
Cited by 8 | Viewed by 1927
Abstract
Tepotinib (MSC2156119) is a potent mesenchymal–epithelial transition (MET) factor inhibitor, a receptor tyrosine kinase that plays a crucial role in promoting cancer cell malignant progression. Adverse effects of tepotinib (TEP), such as peripheral edema, interstitial lung disease, nausea and diarrhea, occur due to [...] Read more.
Tepotinib (MSC2156119) is a potent mesenchymal–epithelial transition (MET) factor inhibitor, a receptor tyrosine kinase that plays a crucial role in promoting cancer cell malignant progression. Adverse effects of tepotinib (TEP), such as peripheral edema, interstitial lung disease, nausea and diarrhea, occur due to drug accumulation and lead to termination of therapy. Therefore, the in silico and experimental metabolic susceptibility of TEP was investigated. In the current work, an LC-MS/MS analytical method was developed for TEP estimation with metabolic stability assessment. TEP and lapatinib (LTP) used as internal standards (ISs) were separated on a reversed-phase C18 column using the isocratic mobile phase. Protein precipitation steps were used to extract TEP from the human liver microsome (HLM) matrix. An electrospray ionization multi-reaction monitoring (MRM) acquisition was conducted at m/z 493→112 for TEP, at m/z 581→350, and 581→365 for the IS. Calibration was in the range of 5 to 500 ng/mL (R2 = 0.999). The limit of detection (LOD) was 0.4759 ng/mL, whereas the limit of quantification (LOQ) was 1.4421 ng/mL. The reproducibility of the developed analytical method (inter- and intra-day precision and accuracy) was within 4.39%. The metabolic stability of TEP in HLM was successfully assessed using the LC-MS/MS method. The metabolic stability assessment of TEP showed intermediate Clint (35.79 mL/min/kg) and a moderate in vitro t1/2 (22.65 min), proposing the good bioavailability and moderate extraction ratio of TEP. The in silico results revealed that the N-methyl piperidine group is the main reason of TEP metabolic lability. The in silico Star Drop software program could be used in an effective protocol to confirm and propose the practical in vitro metabolic experiments to spare resources and time, especially during the first stages for designing new drugs. The established analytical method is considered the first LC-MS/MS method for TEP estimation in the HLM matrix with its application to metabolic stability assessment. Full article
(This article belongs to the Special Issue Application of Liquid Chromatography in Pharmaceutical and Toxicological Analysis)
►▼ Show Figures

Figure 1

Review

Jump to: Research

22 pages, 5053 KiB  
Review
The Application of Liquid Chromatography for the Analysis of Organic UV Filters in Environmental and Marine Biota Matrices
by Maria Nieddu, Valeria Pasciu, Maria Piera Demontis and Elena Baralla
Separations 2024, 11(1), 30; https://doi.org/10.3390/separations11010030 - 12 Jan 2024
Cited by 1 | Viewed by 2087
Abstract
Sunscreens are topical preparations containing one or more compounds that protect humans from ultraviolet (UV) light. This review focuses on analytical methods, particularly liquid chromatography, with the aim of identifying and determining UV filters (UVFs) in environmental and marine biota matrices. A literature [...] Read more.
Sunscreens are topical preparations containing one or more compounds that protect humans from ultraviolet (UV) light. This review focuses on analytical methods, particularly liquid chromatography, with the aim of identifying and determining UV filters (UVFs) in environmental and marine biota matrices. A literature review was conducted using NIH (PubMed and Medline), FDA and EPA databases, Google Scholar, and federal regulations. This retrospective literature review is focused on the last five years. UVF quantification in environmental and biological matrices showed a wide array of methods where liquid chromatography is predominant. The scientific literature identified a large variety of analytical methodologies that are compared in this review to evaluate the better results in terms of limits of quantification and the possibility to identify as many analytes as possible simultaneously. Full article
(This article belongs to the Special Issue Application of Liquid Chromatography in Pharmaceutical and Toxicological Analysis)
16 pages, 1441 KiB  
Review
A Review of Liquid Chromatography-Mass Spectrometry Strategies for the Analyses of Metabolomics Induced by Microplastics
by Kuan-Lu Wu, Wan-Rou Liao, Wei-Chen Lin and Sung-Fang Chen
Separations 2023, 10(4), 257; https://doi.org/10.3390/separations10040257 - 16 Apr 2023
Cited by 2 | Viewed by 2862
Abstract
Microplastics (MPs) (microscopic plastic particles) are defined as plastic fragments in the range of 1 to 5 mm. They are invisible and usually too small to be seen by humans but pollution by MPs has become an issue due to the rising use [...] Read more.
Microplastics (MPs) (microscopic plastic particles) are defined as plastic fragments in the range of 1 to 5 mm. They are invisible and usually too small to be seen by humans but pollution by MPs has become an issue due to the rising use of plastic products. Pollution of microscopic plastics has gained international attention in recent years and has become an important issue in the field of environmental protection, food safety, and human health. Numerous studies have reported that MPs have the potential for causing detrimental effects in various species. The focus of this mini review was on LC-MS-based metabolomics research into this issue by targeted and untargeted approaches. We also summarized biomarkers for assessing toxicity in land and aquatic species that are induced by MPs with different sizes and shapes, type of monomer, and the dose. Based on previous research results, MPs have the potential for affecting energy metabolism and the immune system, chronic inflammation, and neurotransmitter disorders in a wide variety of species. These biomarkers discovered by metabolomics are consistent with other methods, showing the reliability of LC-MS-based metabolomics. Further research is highly anticipated to explore other toxicity effects that are induced by MPs. Full article
(This article belongs to the Special Issue Application of Liquid Chromatography in Pharmaceutical and Toxicological Analysis)
►▼ Show Figures

Figure 1

Show export options expand_more Show export options expand_less
Select all
Export citation of selected articles as:
 
Displaying articles 1-5
Back to TopTop