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The Application of LC-MS in Pharmaceutical Analysis
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The Application of LC-MS in Pharmaceutical Analysis

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: 31 October 2024 | Viewed by 6763

Special Issue Editors

Dr. Wing Lam

E-Mail Website
Guest Editor
Department of Pharmacology, Yale University School of Medicine, 333 Cedar Street, SHM B254, New Haven, CT 06510, USA
Interests: drug-drug interaction analysis; cell signaling; herbal chemcials
Dr. Wei Cai

E-Mail Website
Guest Editor
Deputy Dean of School of Pharmaceutical Sciences and Director of Pharmaceutical Analysis Teaching and Research Office, Hunan University of Medicine, Huaihua 41800, China
Interests: LC-MS; metabolites; pharmaceutical analysis

Special Issue Information

Dear Colleagues,

Over the past few decades, liquid chromatography–mass spectrometry (LC-MS), liquid chromatography–mass spectrometry (LC-MS), and ultra-high-performance liquid chromatography combined with high-resolution mass spectrometry (UHPLC-HRMS) have gained significant prominence as vital analytical instruments, particularly the latter. Their superior separating efficiency, specificity, and sensitivity have rendered them indispensable in various fields, especially in pharmaceutical analysis. Therefore, we propose an in-depth exploration of the applications and advancements of LC-MS in pharmaceutical analysis through a dedicated Special Issue, titled “The application of LC-MS in pharmaceutical analysis”.

This Special Issue aims to gather and disseminate the latest research, methodologies, and findings related to the application of LC-MS in pharmaceutical analysis. We envision a comprehensive collection of manuscripts that cover a wide range of themes, including (but not limited to) the following:

  1. Method development and validation using LC-MS for pharmaceutical analysis;
  2. Chemical characterization and metabolite identification using LC-MS;
  3. Untargeted and targeted metabolomics studies employing LC-MS;
  4. Pharmacokinetic analysis using LC-MS techniques;
  5. High-throughput LC-MS approaches for drug discovery and analysis;
  6. The analysis and identification of impurities and degradation products using LC-MS.

We believe that this Special Issue will serve as an excellent platform for researchers and practitioners in the field to share their valuable insights, novel methodologies, and significant findings. It will not only contribute to the existing knowledge base but also stimulate further advancements in LC-MS technology and its applications in pharmaceutical analysis.

Dr. Wing Lam
Dr. Wei Cai
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. Molecules is an international peer-reviewed open access semimonthly 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 2700 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

  • LC–MS
  • chemical characterization
  • metabolite identification
  • metabolomics
  • pharmacokinetics

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Published Papers (6 papers)

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Research

14 pages, 1000 KiB  
Article
Advancing Bioanalytical Method Validation: A Comprehensive ICH M10 Approach for Validating LC–MS/MS to Quantify Fluoxetine in Human Plasma and Its Application in Pharmacokinetic Studies
by Aimen El Orche, Amine Cheikh, Choukri El Khabbaz, Houda Bouchafra, My El Abbes Faouzi, Yahya Cherrah, Siddique Akber Ansari, Hamad M. Alkahtani, Shoeb Anwar Ansari and Mustapha Bouatia
Molecules 2024, 29(19), 4588; https://doi.org/10.3390/molecules29194588 - 27 Sep 2024
Viewed by 453
Abstract
A fast and sample cleanup approach for fluoxetine in human plasma was developed using protein precipitation coupled with LC–MS-MS. Samples were treated with methanol prior to LC–MS-MS analysis. Chromatographic separation was performed on a reverse phase column with an isocratic mobile phase of [...] Read more.
A fast and sample cleanup approach for fluoxetine in human plasma was developed using protein precipitation coupled with LC–MS-MS. Samples were treated with methanol prior to LC–MS-MS analysis. Chromatographic separation was performed on a reverse phase column with an isocratic mobile phase of methanol and 10 mM ammonium formate pH acidified with formic acid (80:20, v/v) at a flow rate of 0.2 mL/min. The run time was 4 min. Mass parameters were optimized to monitor transitions at m/z [M + H]+ 310 > > 148 for fluoxetine and m/z [M + H]+ 315.1 > > 153 for fluoxetine-d5 as an internal standard. The lower limit of quantification and the dynamic range were 0.25 and 0.25–50 ng/mL, respectively. Linearity was good for intra-day and inter-day validations (R2 = 0.999). The matrix effect was acceptable with CV% < 15 and accuracy% < 15. The hemolytic effect was negligible. Fluoxetine was stable in human plasma for 48 h at room temperature (25 °C), for 12 months frozen at −25 °C, for 48 h in an auto-sampler at 6 °C, and for three freeze/thaw cycles. The validated method was applied in a pharmacokinetic study to determine the concentration of fluoxetine in plasma samples. The study provides a fast and simple bioanalytical method for routine analysis and may be particularly useful for bioequivalence studies. The method was successfully applied to a pharmacokinetic study of fixed-dose fluoxetine in nine healthy volunteers. Full article
(This article belongs to the Special Issue The Application of LC-MS in Pharmaceutical Analysis)
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19 pages, 3154 KiB  
Article
A Systematic Methodology for the Identification of the Chemical Composition of the Mongolian Drug Erdun-Uril Compound Utilizing UHPLC-Q-Exactive Orbitrap Mass Spectrometry
by Yanghui Huo, Kailin Li, Suyu Yang, Bo Yi, Zhihua Chai, Lingxuan Fan, Liangyin Shu, Bowen Gao, Huanting Li and Wei Cai
Molecules 2024, 29(18), 4349; https://doi.org/10.3390/molecules29184349 - 13 Sep 2024
Viewed by 595
Abstract
The traditional Mongolian medicine Erdun-Uril is a conventional combination of 29 herbs commonly used for the treatment of cerebrovascular ailments. It has the effects of reducing inflammation, counteracting oxidative stress, and averting strokes caused by persistent cerebral hypoperfusion. Prior research on Erdun-Uril has [...] Read more.
The traditional Mongolian medicine Erdun-Uril is a conventional combination of 29 herbs commonly used for the treatment of cerebrovascular ailments. It has the effects of reducing inflammation, counteracting oxidative stress, and averting strokes caused by persistent cerebral hypoperfusion. Prior research on Erdun-Uril has predominantly concentrated on its pharmacodynamics and mechanism of action; however, there has been a lack of systematic and comprehensive investigation into its chemical constituents. Therefore, it is crucial to establish an efficient and rapid method for evaluating the chemical constituents of Erdun-Uril. In this study, Erdun-Uril was investigated using UHPLC-Q-Exactive Orbitrap MS combined with parallel reaction monitoring for the first time. Eventually, a total of 237 compounds, including 76 flavonoids, 68 phenolic compounds, 19 alkaloids, 7 amino acids, etc., were identified based on the chromatographic retention time, bibliography data, MS/MS2 information, neutral loss fragments (NLFs), and diagnostic fragment ions (DFIs). And of these, 225 were reported for the first time in this study. This new discovery of these complex components would provide a reliable theoretical basis for the development of pharmacodynamics and quality standards of the Mongolian medicine Erdun-Uril. Full article
(This article belongs to the Special Issue The Application of LC-MS in Pharmaceutical Analysis)
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23 pages, 4695 KiB  
Article
Identification of New Hepatic Metabolites of Miconazole by Biological and Electrochemical Methods Using Ultra-High-Performance Liquid Chromatography Combined with High-Resolution Mass Spectrometry
by Michał Wroński, Jakub Trawiński and Robert Skibiński
Molecules 2024, 29(9), 2160; https://doi.org/10.3390/molecules29092160 - 6 May 2024
Viewed by 839
Abstract
The main objective of this study was to investigate the metabolism of miconazole, an azole antifungal drug. Miconazole was subjected to incubation with human liver microsomes (HLM) to mimic phase I metabolism reactions for the first time. Employing a combination of an HLM [...] Read more.
The main objective of this study was to investigate the metabolism of miconazole, an azole antifungal drug. Miconazole was subjected to incubation with human liver microsomes (HLM) to mimic phase I metabolism reactions for the first time. Employing a combination of an HLM assay and UHPLC-HRMS analysis enabled the identification of seven metabolites of miconazole, undescribed so far. Throughout the incubation with HLM, miconazole underwent biotransformation reactions including hydroxylation of the benzene ring and oxidation of the imidazole moiety, along with its subsequent degradation. Additionally, based on the obtained results, screen-printed electrodes (SPEs) were optimized to simulate the same biotransformation reactions, by the use of a simple, fast, and cheap electrochemical method. The potential toxicity of the identified metabolites was assessed using various in silico models. Full article
(This article belongs to the Special Issue The Application of LC-MS in Pharmaceutical Analysis)
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13 pages, 3380 KiB  
Article
In Silico and In Vivo Pharmacokinetic Evaluation of 84-B10, a Novel Drug Candidate against Acute Kidney Injury and Chronic Kidney Disease
by Man Su, Xianru Liu, Yuru Zhao, Yatong Zhu, Mengqiu Wu, Kun Liu, Gangqiang Yang, Wanhui Liu and Lin Wang
Molecules 2024, 29(1), 159; https://doi.org/10.3390/molecules29010159 - 27 Dec 2023
Cited by 1 | Viewed by 1288
Abstract
Acute kidney injury (AKI) and chronic kidney disease (CKD) have become public health problems due to high morbidity and mortality. Currently, drugs recommended for patients with AKI or CKD are extremely limited, and candidates based on a new mechanism need to be explored. [...] Read more.
Acute kidney injury (AKI) and chronic kidney disease (CKD) have become public health problems due to high morbidity and mortality. Currently, drugs recommended for patients with AKI or CKD are extremely limited, and candidates based on a new mechanism need to be explored. 84-B10 is a novel 3-phenylglutaric acid derivative that can activate the mitochondrial protease, Lon protease 1 (LONP1), and may protect against cisplatin-induced AKI and unilateral ureteral obstruction- or 5/6 nephrectomy [5/6Nx]-induced CKD model. Preclinical studies have shown that 84-B10 has a good therapeutic effect, low toxicity, and is a good prospect for further development. In the present study, the UHPLC-MS/MS method was first validated then applied to the pharmacokinetic study and tissue distribution of 84-B10 in rats. Physicochemical properties of 84-B10 were then acquired in silico. Based on these physicochemical and integral physiological parameters, a physiological based pharmacokinetic (PBPK) model was developed using the PK-Sim platform. The fitting accuracy was estimated with the obtained experimental data. Subsequently, the validated model was employed to predict the pharmacokinetic profiles in healthy and chronic kidney injury patients to evaluate potential clinical outcomes. Cmax in CKD patients was about 3250 ng/mL after a single dose of 84-B10 (0.41 mg/kg), and Cmax,ss was 1360 ng/mL after multiple doses. This study may serve in clinical dosage setting in the future. Full article
(This article belongs to the Special Issue The Application of LC-MS in Pharmaceutical Analysis)
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18 pages, 9893 KiB  
Article
Untargeted and Targeted Metabolomics Reveal the Active Peptide of Eupolyphaga sinensis Walker against Hyperlipidemia by Modulating Imbalance in Amino Acid Metabolism
by Yanan Li, Pingping Dong, Long Dai and Shaoping Wang
Molecules 2023, 28(20), 7049; https://doi.org/10.3390/molecules28207049 - 12 Oct 2023
Cited by 1 | Viewed by 1300
Abstract
The active peptide (APE) of Eupolyphaga sinensis Walker, which is prepared by bioenzymatic digestion, has significant antihyperlipidemic effects in vivo, but its mechanism of action on hyperlipidemia is not clear. Recent studies on amino acid metabolism suggested a possible link between it and [...] Read more.
The active peptide (APE) of Eupolyphaga sinensis Walker, which is prepared by bioenzymatic digestion, has significant antihyperlipidemic effects in vivo, but its mechanism of action on hyperlipidemia is not clear. Recent studies on amino acid metabolism suggested a possible link between it and hyperlipidemia. In this study, we first characterized the composition of APE using various methods. Then, the therapeutic effects of APE on hyperlipidemic rats were evaluated, including lipid levels, the inflammatory response, and oxidative stress. Finally, the metabolism-regulating mechanisms of APE on hyperlipidemic rats were analyzed using untargeted and targeted metabolomic approaches. The results showed that APE significantly reduced the accumulation of fat, oxidative stress levels, and serum pro-inflammatory cytokine levels. Untargeted metabolomic analysis showed that the mechanism of the hypolipidemic effect of APE was mainly related to tryptophan metabolism, phenylalanine metabolism, arginine biosynthesis, and purine metabolism. Amino-acid-targeted metabolomic analysis showed that significant differences in the levels of eight amino acids occurred after APE treatment. Among them, the expression of tryptophan, alanine, glutamate, threonine, valine, and phenylalanine was upregulated, and that of arginine and proline was downregulated in APE-treated rats. In addition, APE significantly downregulated the mRNA expression of SREBP-1, SREBP-2, and HMGCR. Taking these points together, we hypothesize that APE ameliorates hyperlipidemia by modulating amino acid metabolism in the metabolome of the serum and feces, mediating the SREBP/HMGCR signaling pathway, and reducing oxidative stress and inflammation levels. Full article
(This article belongs to the Special Issue The Application of LC-MS in Pharmaceutical Analysis)
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24 pages, 9890 KiB  
Article
Comprehensive Metabolite Identification of Genipin in Rats Using Ultra-High-Performance Liquid Chromatography Coupled with High Resolution Mass Spectrometry
by Zhifeng Cui, Zhe Li, Weichao Dong, Lili Qiu, Jiayu Zhang and Shaoping Wang
Molecules 2023, 28(17), 6307; https://doi.org/10.3390/molecules28176307 - 29 Aug 2023
Cited by 1 | Viewed by 1257
Abstract
Genipin, an aglycone of geniposide, is a rich iridoid component in the fruit of Gardenia jasminoides Ellis and has numerous biological activities. However, its metabolic profiles in vivo and vitro remain unclear. In this study, an effective analytical strategy based on ultra-high-performance liquid [...] Read more.
Genipin, an aglycone of geniposide, is a rich iridoid component in the fruit of Gardenia jasminoides Ellis and has numerous biological activities. However, its metabolic profiles in vivo and vitro remain unclear. In this study, an effective analytical strategy based on ultra-high-performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) in positive and negative ion modes was developed to analyze and identify genipin metabolites in rat urine, blood, feces, and fecal fermentation in combination with many methods including post-collection data mining methods, high-resolution extracted ion chromatography (HREIC), and multiple mass defect filtering (MMDF). Simultaneously, the metabolites of genipin in vivo were verified by fecal fermentation of SD rats at different times. Finally, based on information such as reference substances, chromatographic retention behavior, and accurate mass determination, a total of 50 metabolites (including prototypes) were identified in vivo. Among them, 7, 31 and 28 metabolites in vivo were identified in blood, urine, and feces, respectively. Our results showed that genipin could generate different metabolites that underwent multiple metabolic reactions in vivo including methylation, hydroxylation, dehydroxylation, hydrogenation, sulfonation, glucuronidation, demethylation, and their superimposed reactions. Forty-six metabolites were verified in vitro. Meanwhile, 2 and 19 metabolites identified in blood and urine were also verified in fecal fermentation at different times. These results demonstrated that metabolites were produced in feces and reabsorbed into the body. In conclusion, the newly discovered metabolites of genipin can provide a new perspective for understanding its pharmacological effects and build the foundation for thee toxicity and safety evaluations of genipin. Full article
(This article belongs to the Special Issue The Application of LC-MS in Pharmaceutical Analysis)
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