A simple, precise, accurate, robust chiral high-performance liquid chromatographic (chiral HPLC) method was developed for estimation of (S)-piperidin-3-amine (S-isomer) in (R)-piperidin-3-amine dihydrochloride (R-AMP). As AMP is a high-melting solid and nonchromophoric compound, development of a suitable chiral method is a challenging task. The proposed chiral HPLC-UV method involves a precolumn derivatization technique with para toluene sulphonyl chloride (PTSC) in the presence of a base to introduce chromophore into analytes. It utilizes chiralpak AD-H column with a simple mobile phase of 0.1% diethyl amine in ethanol with a 0.5 mL/min flow rate. Analytes were monitored by using a UV detector at 228 nm. The resolution between the two enantiomers was more than 4.0. The developed method was validated as per current International Conference on Harmonization (ICH) guidelines.
Download full-text PDF |
Source |
|---|---|
| http://dx.doi.org/10.1002/chir.22352 | DOI Listing |
Publication Analysis
Top Keywords
Similar Publications
On the Influence of Additives and Modifiers on the Chiral HPLC Separation of the Enantiomers of Nicotine.
Chirality
February 2025
Daicel Chiral Technologies, West Chester, Pennsylvania, USA.
The influence of additives and modifiers on the chiral HPLC separation of the nicotine enantiomers using UV/Vis detection is discussed. Selected alcohols as modifiers and selected amines as additives were found to have a significant effect on the resolution and retention times of nicotine enantiomers even to the point of eliminating component elution. Systematic variations in the concentration of ethanol, methanol, and isopropanol, as modifiers, along with variations in the concentration of diethylamine, triethylamine, tributylamine, ethylenediamine, isopropylamine, as additives, revealed that the average resolution (R) of the nicotine enantiomers ranged from 2.
View Article and Find Full Text PDFDevelopment of a Combined 2D-MGD TLC/HPTLC Method for the Separation of Terpinen-4-ol and α-Terpineol from Tea Tree, , Essential Oil.
Biomolecules
January 2025
United States Department of Agriculture-Agricultural Research Service (USDA-ARS), Subtropical Horticulture Research Station (SHRS), Miami, FL 33158, USA.
Tea tree oil (TTO), acquired from (Maiden & Betche) Cheel, Myrtaceae, is a widely utilized essential oil (EO) due to its bioactive properties. The identification and quantification of TTO ingredients is generally performed by GC-MS, which provides the most accurate results. However, in some instances, the cost and time of analysis may pose a challenge.
View Article and Find Full Text PDFEnantiodifferentiation of Thiohydantoin Derivatives by NMR in the Presence of Chiral Solvating Agent: (1R,2S)-Ephedrine and Chiral Symmetrical and Unsymmetrical Thioureas.
Chirality
February 2025
Department of Chemistry, Bogazici University, Istanbul, Turkey.
2-Thiohydantoin derivatives, including different substitutions at N-1 and C-5 (5-methyl-, 5-isopropyl-, 1-acetyl-5-methyl-, and 1-acetyl-5-isopropyl-) (1-4, respectively), were synthesized by the known literature methods. In these synthetic pathways, it was reported that enantiomerically pure 2-thiohydantions were obtained in the absence of any solvent via the reaction of L-amino acids with thiourea (1&2) and via the reaction of L-amino acids with NHSCN and acetic anhydride (3&4). However, in this study, in contrary to the previous literature studies, racemic mixtures of 2-thiohydantoins were obtained although the same synthetic methods were used.
View Article and Find Full Text PDFStereoselectivity of evodiamine enantiomers in neuroprotective activity, pharmacokinetics and the ability across the blood-brain barrier.
J Chromatogr A
January 2025
School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, PR China. Electronic address:
Evodiamine, a chiral quinazoline alkaloid in the traditional Chinese medicine Evodiae fructus, exhibited efficacy for CNS diseases. In this study, the pure enantiomers of evodiamine were prepared in large quantities via chemical resolution. Their structures were elucidated by MS, NMR and ECD.
View Article and Find Full Text PDFA new stability indicating HPLC method with QDa and PDA detectors for the determination of process and degradation impurities of ivabradine including separation of diastereomeric -oxides.
Anal Methods
January 2025
Istanbul University, Faculty of Pharmacy, Department of Analytical Chemistry, 34116, Istanbul, Turkey.
In this study, a new reversed phase high performance liquid chromatography method using two detectors was developed for the analysis of degradation and process impurities of ivabradine in pharmaceutical preparations. A PDA detector set to 285 nm wavelength and a QDa detector set to positive scan mode were used in the method. In the developed method, the separation process was carried out in a Zorbax phenyl column with a gradient application of a 0.
View Article and Find Full Text PDFWant AI Summaries of new PubMed Abstracts delivered to your In-box?
Enter search terms and have AI summaries delivered each week - change queries or unsubscribe any time!