L‐Cysteine‐Bonded Polymeric Monolithic Stationary Phase for Enantioseparation of Dansyl Amino Acids in Capillary Liquid Chromatography DOI
Ayu Rahayu Anggraeni, Lee Wah Lim,

Toyohide Takeuchi

et al.

Journal of Separation Science, Journal Year: 2024, Volume and Issue: 47(21)

Published: Nov. 1, 2024

A chiral monolith stationary phase was fabricated by modifying the surface using L-cysteine through a thiol-epoxy click reaction. L-cysteine-bonded polymer characterized scanning electron microscopy/energy-dispersive X-ray and attenuated total reflectance Fourier-transformed infrared. The monomer content modification temperature were carefully optimized to create with excellent mechanical stability permeability. Our findings revealed that column morphology depended significantly on porogen concentration for its efficiency. Adequate pores binding sites formed optimal content, while higher improved yield, enhancing peak shapes increasing separation demonstrated capability enantioseparation of dansyl glutamic acid, aspartic methionine, phenylalanine 60 mM ammonium acetate buffer solution acetonitrile in 20:80 v/v ratio. It maintained good repeatability no relative standard deviation exceeding 7%. These results indicated has potential as phase.

Language: Английский

Recent Advances in Enantiorecognition and Enantioseparation Techniques of Chiral Molecules in the Pharmaceutical Field DOI Open Access

Kuladip Barman,

Md. Shafiqul Islam, Kalyan Kumar Das

et al.

Biomedical Chromatography, Journal Year: 2025, Volume and Issue: 39(2)

Published: Jan. 2, 2025

ABSTRACT Enantioseparation and enantiorecognition are crucial in the pharmaceutical analysis of chiral substances, impacting safety, efficacy, regulatory compliance. refers to process separating enantiomers from a mixture, typically achieved through chromatography techniques like HPLC SFC. In contrast, involves identification based on their interaction with selector without need for separation. Recent advancements these have significantly improved enantioseparation efficiency resolution. Chiral stationary phases (CSPs) evolved, offering better selectivity, including hybrid organic–inorganic materials miniaturization. The use green solvents has also reduced environmental impact. Non‐chromatographic methods, such as circular dichroism (CD) nuclear magnetic resonance (NMR) spectroscopy, enable interactions polarized light or solvents. However, methods face challenges, high costs, limited solvent compatibility, shorter operational lifespans compared chromatographic techniques. developments solvent‐tolerant CSPs aim address limitations. This review highlights innovations, focusing relevance industry, pollution control, quality assurance, emphasizes growing importance production regulation drugs.

Language: Английский

Citations

1
Room temperature synthesis of a chiral covalent organic framework core‐shell composite for high‐performance liquid chromatography enantioseparation DOI
Yue Zhang,

Yan‐Rui Lu,

Cheng Liu

et al.

Journal of Separation Science, Journal Year: 2024, Volume and Issue: 47(15)

Published: Aug. 1, 2024

In this article, chiral covalent organic framework core-shell composite CCOF-TpPa-Py@SiO

Language: Английский

Citations

4
Indirect chromatographic approach for enantioselective analysis of chiral environmental pollutants DOI

Michael Lämmerhofer

Comprehensive analytical chemistry, Journal Year: 2025, Volume and Issue: unknown

Published: Jan. 1, 2025

Language: Английский

Citations

0
Chiral Separation of pharmaceuticals and agrochemicals using capillary electrophoresis: Migration order, modeling and chiral recognition mechanism DOI
Ann Gogolashvili,

Elene Tatunashvili,

Lali Chankvetadze

et al.

Talanta, Journal Year: 2025, Volume and Issue: unknown, P. 128004 - 128004

Published: March 1, 2025

Language: Английский

Citations

0
Tetraphenylethylene based Chiral AIEgen for Enantioselective Detection of Chiral Acids DOI
Chunxuan Qi, Qingyang Li,

Keyue Wei

et al.

Dyes and Pigments, Journal Year: 2025, Volume and Issue: unknown, P. 112781 - 112781

Published: March 1, 2025

Language: Английский

Citations

0
CHIRAL ANALYSIS BY CAPILLARY ELECTROMIGRATION TECHNIQUES DOI
Samuel Bernardo‐Bermejo,

Sandra Adámez-Rodríguez,

María Castro‐Puyana

et al.

TrAC Trends in Analytical Chemistry, Journal Year: 2025, Volume and Issue: unknown, P. 118256 - 118256

Published: April 1, 2025

Language: Английский

Citations

0
Enantioseparation of Mirabegron Using Cyclodextrin‐based Chiral Columns: High‐performance Liquid Chromatography and Molecular Modeling Study DOI Creative Commons

Ali Mhammad,

Gergely Dombi,

Máté Dobó

et al.

Journal of Separation Science, Journal Year: 2025, Volume and Issue: 48(4)

Published: April 1, 2025

ABSTRACT A novel high‐performance liquid chromatography method for the enantioseparation of mirabegron ( R ‐mirabegron), a selective β‐3 adrenergic receptor agonist, using cyclodextrin (CD)‐based chiral stationary phases (CSPs) was developed. Seven different CSPs containing β‐, γ‐, hydroxypropyl‐β‐, sulfobutyl‐β‐, carboxymethyl‐β‐, permethyl‐β‐, and phenylcarbamate‐β‐cyclodextrin were evaluated under both polar organic reversed‐phase conditions. Only Chiral CD‐Ph column displayed enantiorecognition. Optimization conditions full factorial design led to determination most suitable conditions: mobile phase composition 90:10:0.1 methanol:water:diethylamine, flow rate 0.8 mL/min, temperature 40°C with enantiomeric elution order, where impurity S ‐mirabegron elutes first. Using optimized conditions, s = 1.9 achieved within 10 min. The developed validated according current guidelines successfully applied ‐mirabegron, as in pharmaceutical formulations. enantiorecognition mechanism investigated by molecular docking thermodynamic analysis. modeling, interactions between CDs analyte analyzed at level, revealing that interacts primarily phenylcarbamate groups on outer surface structure. Enthalpy‐controlled consistently observed across all eluent compositions, regardless is highly routine purity mirabegron, offering reliable tool regulatory compliance.

Language: Английский

Citations

0
Determination of Enantiomeric Impurity in Tegoprazan Drug Substance by HPLC DOI
Lei Zhang,

Shutao Duan,

Shujuan Xu

et al.

Separation Science Plus, Journal Year: 2024, Volume and Issue: 7(11)

Published: Aug. 25, 2024

ABSTRACT Tegoprazan is a novel potassium‐competitive acid blocker used for gastroesophageal reflux disease. It administered as the ( S )‐ and R )‐enantiomers are considered impurities that should be controlled. The objective of this work was to establish chiral analytical method determination enantiomeric impurity tegoprazan in drug substance by high‐performance liquid chromatography (HPLC). Enantioselective separation performed on Chiralpak alpha1‐acid glycoprotein (AGP) column (4.6 mm × 250 mm, 5.0 µm) at 30°C utilizing mobile phase consisting 5 mmol L −1 ammonium acetate buffer (pH 6.0) 2‐propanol (93:7, v/v) flow rate 0.7 mL min with detection wavelength 220 nm. effects chromatographic conditions, including type concentration organic modifiers, pH, concentration, rate, temperature, were thoroughly investigated. Under optimized resolution between )‐tegoprazan greater than 3.0. Moreover, developed validated terms linearity, limits (LOD) quantitation (LOQ), accuracy, precision, stability. Each enantiomer showed good linear relationship over range 1.0–100 µg , correlation coefficient 0.9999. LOD LOQ 0.1 0.3 respectively. In addition, recoveries ranged from 94.10% 99.39% relative standard deviation (RSD) 1.9%. Application proposed determine proved satisfactory. quantitative results about 2.0%, demonstrating remained controlled quality criteria.

Language: Английский

Citations

0
L‐Cysteine‐Bonded Polymeric Monolithic Stationary Phase for Enantioseparation of Dansyl Amino Acids in Capillary Liquid Chromatography DOI
Ayu Rahayu Anggraeni, Lee Wah Lim,

Toyohide Takeuchi

et al.

Journal of Separation Science, Journal Year: 2024, Volume and Issue: 47(21)

Published: Nov. 1, 2024

A chiral monolith stationary phase was fabricated by modifying the surface using L-cysteine through a thiol-epoxy click reaction. L-cysteine-bonded polymer characterized scanning electron microscopy/energy-dispersive X-ray and attenuated total reflectance Fourier-transformed infrared. The monomer content modification temperature were carefully optimized to create with excellent mechanical stability permeability. Our findings revealed that column morphology depended significantly on porogen concentration for its efficiency. Adequate pores binding sites formed optimal content, while higher improved yield, enhancing peak shapes increasing separation demonstrated capability enantioseparation of dansyl glutamic acid, aspartic methionine, phenylalanine 60 mM ammonium acetate buffer solution acetonitrile in 20:80 v/v ratio. It maintained good repeatability no relative standard deviation exceeding 7%. These results indicated has potential as phase.

Language: Английский

Citations

0