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Separations
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Application of Chromatography in Pharmaceutical and Biomedical Analysis
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Application of Chromatography in Pharmaceutical and Biomedical Analysis

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

Deadline for manuscript submissions: closed (31 July 2023) | Viewed by 12390

Special Issue Editors

Dr. Mohd Abul Kalam

E-Mail Website
Guest Editor
Department of Pharmaceutics, College of Pharmacy, King Saud University, Riyadh, Saudi Arabia
Interests: formulation development; drug delivery; polymeric nanoparticles; nanomedicine; analytical and bioanalytical method development; biopharmaceutics
Prof. Dr. Perwez Alam

E-Mail Website
Guest Editor
Department of Pharmacognosy, College of Pharmacy, King Saud University, Riyadh, Saudi Arabia
Interests: natural product isolation; phytochemical analysis; biological activities; extraction of herbal drugs; stability study; quality control of herbal drugs

Special Issue Information

Dear Colleagues,

Chromatographic analyses, including high-performance liquid chromatography (HPLC), ultra-performance liquid chromatography, and liquid chromatography–mass spectrometry (LC-MS/MS), are powerful and generally applicable for the separation, identification, quantification, and determination of chemical substances in complex mixtures in different samples, including biological fluids. Chromatography can separate and detect a wide range of substances, from ions to compounds, from small molecules to biomolecules, from nonpolar to polar molecules, from non-volatile to volatile substances, and from samples of interest to internal standards used during the analysis of biological samples.

The applications of chromatography have grown explosively in recent decades, due not only to the development of new types of chromatographic techniques including pharmacokinetic (bioavailability) analysis but also to the growing need for characterizing complex mixtures and complex samples. Chromatography has become a powerful tool for qualitative identification and quantitative determination in areas such as biological analysis, pharmaceutical and biomedical analysis, food analysis, environmental analysis, clinical sample analysis, and so on.

This Special Issue of Separations entitled “Application of Chromatography in Pharmaceutical and Biomedical Analysis” will present the latest research, advancements, and applications. This Special Issue accepts research papers and critical reviews on all aspects of applications of chromatography.

Dr. Mohd Abul Kalam
Prof. Dr. Perwez Alam
Guest Editors

Manuscript Submission Information

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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

  • chromatography
  • HPLC/ UPLC
  • HPTLC
  • LC-MS/MS
  • stability sample analysis
  • pharmaceutical analysis
  • biological analysis
  • biopharmaceutical analysis
  • biomedical analysis
  • pharmacokinetics of drugs

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Published Papers (4 papers)

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Research

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16 pages, 2377 KiB  
Article
Development and Validation of UPLC–MS/MS Method for Quantitative Analysis of 5-Fluorouracil in Aqueous Humor of Rabbits
by Mohd Abul Kalam, Sulaiman S. Alhudaithi, Adel Ali Alhowyan, Muzaffar Iqbal, Mohammad Raish, Abdullah K. Alshememry, Musaed Alkholief, Aliyah A. Almomen and Aws Alshamsan
Separations 2023, 10(6), 343; https://doi.org/10.3390/separations10060343 - 2 Jun 2023
Viewed by 1770
Abstract
5-Fluorouracil (5-FU) is now used in eye drops for the management of conjunctival malignant melanoma, intraepithelial neoplasia, and corneal and conjunctival squamous cell carcinoma. The previously used methods for 5-FU quantification in AqH were time-consuming and less sensitive. Herein, a highly perceptive bioanalytical [...] Read more.
5-Fluorouracil (5-FU) is now used in eye drops for the management of conjunctival malignant melanoma, intraepithelial neoplasia, and corneal and conjunctival squamous cell carcinoma. The previously used methods for 5-FU quantification in AqH were time-consuming and less sensitive. Herein, a highly perceptive bioanalytical UPLC–MS/MS method was developed for the quantitative determination of 5-FU in the aqueous humor (AqH) of rabbits using allopurinol as the internal standard (IS). The 5-FU and IS were well separated in an Acquity™ HILIC column. Acetonitrile and 10 mM of ammonium acetate at 95:5 (v/v) were isocratically pumped at a 0.3 mL/min flow rate with a total runtime of 2.5 min. AqH samples were processed with a liquid–liquid extraction method in ethyl acetate. The 5-FU and IS were identified in the negative mode with electrospray ionization. The parent to daughter ion transitions for the 5-FU and IS occurred at m/z 128.92→41.68 and 134.80→64.10, respectively, as quantified using the multiple reaction monitoring mode. The developed method was validated with the ICH-Harmonized Guideline for Bioanalytical Method Validation, and the parameters were within acceptable limits. The calibration curve was linear at the 10.5–2000 ng/mL concentration range, with a correlation coefficient (R2) of 0.9946, and the lower limit of detection was 3.55 ng/mL. The developed and validated method was rapid, sensitive, accurate and robustly able to quantify 5-FU in rabbit AqH. The method was effectively applied to establish the ocular pharmacokinetics of 5-FU following the topical instillation of 5-FU-containing preparations in rabbits. Full article
(This article belongs to the Special Issue Application of Chromatography in Pharmaceutical and Biomedical Analysis)
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19 pages, 4788 KiB  
Article
Rilpivirine and Dolutegravir Simultaneously Measured via RP-HPLC-PDA with Box–Behnken Design Application: A Study of Forced Degradation under Various Conditions
by Shadma Wahab, Mohammad Khalid, Sarfaraz Ahmad and Sherouk Hussein Sweilam
Separations 2023, 10(3), 185; https://doi.org/10.3390/separations10030185 - 8 Mar 2023
Cited by 2 | Viewed by 1898
Abstract
Simultaneous estimation of rilpivirine (RLVN) and dolutegravir (DTGR) in bulk and tablet dosage forms via RP-HPLC-PDA with a Box–Behnken design (BBD) has been performed in this study to develop a fast, precise, timely and cost-saving method for estimating RLVN and DTGR in bulk [...] Read more.
Simultaneous estimation of rilpivirine (RLVN) and dolutegravir (DTGR) in bulk and tablet dosage forms via RP-HPLC-PDA with a Box–Behnken design (BBD) has been performed in this study to develop a fast, precise, timely and cost-saving method for estimating RLVN and DTGR in bulk and tablet dosage forms. The chromatographic conditions were optimized via the BBD, and the developed method was validated according to the ICH guidelines. Additionally, forced degradation studies were also conducted. RLVN and DTGR peaks were observed at retention times of 2.167 and 2.716 min, respectively, in a 6-min runtime. Kromasil 150 mm× 4.6 mm, 5 µm C 18 column was used. The flow rate of the mobile phase was 1.0 mL/min at a temperature of 30 °C. The mobile phase composition was a 0.1% OPA buffer and acetonitrile (ACN) in a 60:40 ratio. Elutes were measured at 260 nm (max) after being injected in a sample volume of 10 µL. The assay result of the marketed tablet was 99.19% and 99.09% for RLVN and DTGR, respectively. The results of forced degradation studies in different chemical environments conditions such as acid, base, dry heat, photo-stability, neutral, and oxidation conditions were observed for RLVN (5.96, 4.79, 3.27, 2.36, 0.99, and 4.35 in percentage degradation) and DTGR (5.67, 4.44, 4.09, 1.81, 0.43, and 4.28 in percentage degradation). The results of the validation parameters were within an acceptable range. The newly formed RP-HPLC-PDA method is novel, fast, precise, time-saving, and cost-effective. Full article
(This article belongs to the Special Issue Application of Chromatography in Pharmaceutical and Biomedical Analysis)
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11 pages, 4112 KiB  
Article
Pharmacognostical and Phytochemical Evaluation of a Unani Polyherbal Formulation: Dawa ul Kurkum by HPTLC
by Meenakshi Gupta, Sajida Sumaiya, Sher Ali, Tanveer Naved, Archana Sharma, Ajaz Ahmad, Mohammed Sikander and Maryam Sarwat
Separations 2023, 10(2), 89; https://doi.org/10.3390/separations10020089 - 28 Jan 2023
Cited by 4 | Viewed by 3322
Abstract
Background: Dawa ul Kurkum (Duk) is a widely used Unani formulation. It consists of seven plant herbs, including stigmas of Crocus sativus L., rhizomes of Nardostachys jatamansi (D.Don) DC., the bark of Cinnamomum cassia (L.) J. Presl., shoot of Cymbopogon jwarancusa (Jones ex [...] Read more.
Background: Dawa ul Kurkum (Duk) is a widely used Unani formulation. It consists of seven plant herbs, including stigmas of Crocus sativus L., rhizomes of Nardostachys jatamansi (D.Don) DC., the bark of Cinnamomum cassia (L.) J. Presl., shoot of Cymbopogon jwarancusa (Jones ex Roxb.) Schult., the resin of Commiphora wightii (Arn.) Bhandari, roots of Saussurea lappa (Decne.) Sch.Bip., and bark of Cinnamomum zeylanicum Blume. However, no study has been previously conducted to characterize this formulation. Thus, the present study was designed to carry out the pharmacognostic and phytochemical characterization of Duk. Methods: Duk was prepared following the protocols in Bayaz e Kabeer and The National Formulary of Unani Medicine Part-I. The characterization included organoleptic properties, fluorescence analysis, preliminary phytochemical screening, antioxidant activity, and active constituent profiling using HPTLC. Results: Evaluation of Duk showed the presence of carbohydrates, flavonoids, quinones, glycosides, cardiac glycosides, terpenoids, phenols, coumarin, steroids, and phytosterols. The total phenolic and flavonoid content was 5.75 ± 0.23 mg GAE/g and 10 ± 0.18 mg QUE/g, respectively. HPTLC of Duk showed the presence of p-coumaric acid, cinnamaldehyde, citral, crocin, isovaleric acid, guggulsterone, and dehydrocostus lactone. Conclusions: Our findings supported the use of Duk as a conventional medicine, and these results could be used as a reference for the standardization of Duk. Full article
(This article belongs to the Special Issue Application of Chromatography in Pharmaceutical and Biomedical Analysis)
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Review

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24 pages, 697 KiB  
Review
Carnosic Acid and Carnosol: Analytical Methods for Their Determination in Plants, Foods and Biological Samples
by Christiana Mantzourani, Petros A. Tarantilis and Maroula G. Kokotou
Separations 2023, 10(9), 481; https://doi.org/10.3390/separations10090481 - 2 Sep 2023
Cited by 2 | Viewed by 4706
Abstract
Among the various phytochemicals, which are present in Lamiaceae plants, carnosic acid and carnosol stand out. Carnosic acid is a phenolic diterpene carrying two phenolic hydroxyl groups and a carboxyl group, while carnosol carries a lactone moiety in addition to phenolic hydroxyls. Both [...] Read more.
Among the various phytochemicals, which are present in Lamiaceae plants, carnosic acid and carnosol stand out. Carnosic acid is a phenolic diterpene carrying two phenolic hydroxyl groups and a carboxyl group, while carnosol carries a lactone moiety in addition to phenolic hydroxyls. Both these phenolic diterpenes exhibit interesting biological properties, such as antioxidant, anticancer, anti-inflammatory and neuroprotective activities. In this review, we summarize the existing analytical methods for the determination of carnosic acid and carnosol, primarily in plants, but also in foods and biological samples. Due to the biological importance of carnosic acid and carnosol, a variety of analytical methods, including high-performance liquid chromatography–ultra violet (HPLC–UV), liquid chromatography–mass spectrometry (LC–MS) and capillary electrophoresis (CE), were developed for their determination. In addition, we discuss the extraction methods applied for their isolation from plants and in brief the bioactivities of these phytochemicals. Full article
(This article belongs to the Special Issue Application of Chromatography in Pharmaceutical and Biomedical Analysis)
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