scholarly journals Direct Chiral HPLC Method for the Simultaneous Separation of Ezetimibe and Tramadol Enantiomers Using a Polysaccharide Stationary Phase

2016 ◽  
Vol 2 (3) ◽  
pp. 1-5
Author(s):  
Sathiyasundar Ramalingama ◽  
Selvakumar Kanthiah ◽  
Valliappan Kannappan
Keyword(s):  
Stationary Phase ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Simultaneous Separation

Enantioseparation of Eight Pairs of Tetralone Derivative Enantiomers on Cellulose Based Chiral Stationary Phase by HPLC

2020 ◽  
Vol 16 (5) ◽  
pp. 539-547
Author(s):  
Qiongwen Zhang ◽  
Junyuan Zhang ◽  
Xia Wang ◽  
Jia Yu ◽  
Xingjie Guo
Keyword(s):  
Stationary Phase ◽  
Normal Mode ◽  
Chiral Stationary Phase ◽  
Hplc Method ◽  
New Drugs ◽  
Phase System ◽  
Chiral Hplc ◽  
Column Temperature ◽  
Chiralpak Ic

Background: Tetralone derivatives, important resources for the development of new drugs which can act in the treatment of central nervous system disorders or participate in synthesis reaction for the synthesis of various pharmaceuticals, have great research value and a bright prospect in exploitation. Methods: A novel chiral HPLC method for efficient enantioseparation of eight tetralone derivative enantiomers was developed on cellulose based CHIRALPAK IC chiral stationary phase under normal mode by investigating the effects of type and content of organic modifier, column temperature and flow rate on retention and enantioselectivity. Besides, the specificity, linearity, stability, precision, accuracy and robustness of this method were also validated. Results: Satisfactory enantioseparation was obtained for all enantiomers in n-hexane/2-propanol mobile phase system at ambient temperature. The thermodynamic study indicated that the solute transfer from the mobile to stationary phase was enthalpically favorable, and the process of enantioseparation was mainly enthalpy controlled. This method met the requirements for quantitative determination of tetralone derivative enantiomers. Conclusion: This study can provide great and important application value for enantioseparation of eight pairs of newly synthesized tetralone derivative enantiomers under normal mode using CHIRALPAK IC chiral column.

A validated chiral HPLC method for the enantiomeric separation of Linezolid on amylose based stationary phase

2003 ◽  
Vol 32 (1) ◽  
pp. 21-28 ◽  
Author(s):  
Ch. Lakshmi Narayana ◽  
T. Suresh ◽  
S. Mahender Rao ◽  
P.K. Dubey ◽  
J. Moses Babu
Keyword(s):  
Stationary Phase ◽  
Enantiomeric Separation ◽  
Hplc Method ◽  
Chiral Hplc

Development and Validation of the Chiral HPLC Method for Daclatasvir in Gradient Elution Mode on Amylose-Based Immobilized Chiral Stationary Phase

2016 ◽  
Vol 79 (21-22) ◽  
pp. 1457-1467 ◽  
Author(s):  
G. Srinivasu ◽  
K. Nagesh Kumar ◽  
Ch. Thirupathi ◽  
Ch. Lakshmi Narayana ◽  
Ch. Parameswara Murthy
Keyword(s):  
Stationary Phase ◽  
Chiral Stationary Phase ◽  
Gradient Elution ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Development And Validation ◽  
Gradient Elution Mode

scholarly journals Simultaneous determination of clobutinol hydrochloride and doxylamine succinate from syrups by RP HPLC using a new stationary phase containing embedded urea polar groups

2012 ◽  
Vol 48 (2) ◽  
pp. 315-323 ◽  
Author(s):  
Paulo Cesar Pires Rosa ◽  
Isabel Cristina Sales Fontes Jardim
Keyword(s):  
Stationary Phase ◽  
Simultaneous Determination ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Polar Groups ◽  
Ich Guidelines ◽  
Relative Standard ◽  
New Stationary Phase

A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO) and doxylamine succinate (DOX) in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size) synthetized at the Liquid Chomatography Laboratory (LabCrom) of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5) in the gradient mode. The diode array detector (DAD) was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD) less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX) over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX). The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.

scholarly journals Characterization of the synthetic cannabinoid MDMB-CHMCZCA

2016 ◽  
Vol 12 ◽  
pp. 2808-2815 ◽  
Author(s):  
Carina Weber ◽  
Stefan Pusch ◽  
Dieter Schollmeyer ◽  
Sascha Münster-Müller ◽  
Michael Pütz ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Hplc Method ◽  
Enantiomeric Purity ◽  
Synthetic Cannabinoid ◽  
Spectroscopic Techniques ◽  
Chiral Hplc ◽  
Tandem Mass ◽  
Synthetic Sample

The synthetic cannabinoid MDMB-CHMCZCA was characterized by various spectroscopic techniques including NMR spectroscopy and tandem mass spectrometry. The synthetic sample was found to be of S-configuration by VCD spectroscopy and comparison of the data with DFT calculations, while ECD spectroscopy was found to be inconclusive in this case. The enantiomeric purity of samples from test purchases and police seizures was assessed by a self-developed chiral HPLC method.

Simultaneous separation of hydrophobic and hydrophilic peptides with a silica hydride stationary phase using aqueous normal phase conditions

2011 ◽  
Vol 1218 (44) ◽  
pp. 8021-8026 ◽  
Author(s):  
Reinhard I. Boysen ◽  
Yuanzhong Yang ◽  
Jamil Chowdhury ◽  
Maria T. Matyska ◽  
Joseph J. Pesek ◽  
...  
Keyword(s):  
Stationary Phase ◽  
Normal Phase ◽  
Simultaneous Separation ◽  
Silica Hydride ◽  
Aqueous Normal Phase

Monolithic stationary phase coupled with coulometric detection: Development of an ion-pair HPLC method for the analysis of quinone-bearing compounds

2007 ◽  
Vol 30 (17) ◽  
pp. 2935-2942 ◽  
Author(s):  
Francesca Mancini ◽  
Maria L. Bolognesi ◽  
Carlo Melchiorre ◽  
Andrea Cavalli ◽  
Vincenza Andrisano
Keyword(s):  
Stationary Phase ◽  
Hplc Method ◽  
Ion Pair ◽  
Coulometric Detection ◽  
Monolithic Stationary Phase

scholarly journals Reverse Phase Chiral HPLC Method for Enantiomeric Excess Determination of 2-Aminobutanamide

2019 ◽  
Vol 32 (1) ◽  
pp. 69-72
Author(s):  
T. Naga Jhansi ◽  
D. Pavan Kumar ◽  
Nagaraju Rajana ◽  
D. Jayadeep Kumar ◽  
G. Nageswara Rao
Keyword(s):  
Limit Of Detection ◽  
Enantiomeric Excess ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Perchloric Acid Solution ◽  
Column Temperature ◽  
Isomer Content

A reverse phase chiral HPLC method was developed for the determination of (R)-2-aminobutanamide isomer content in (S)-2-amino-butanamide key starting material for levetiracetam drug substance by using a CROWNPAK CR (+) column. Perchloric acid solution (0.05 %) was used as mobile phase and the flow rate was finalized as 0.3 mL/min. UV detection wavelength was 200 nm and column temperature was set as 15 ºC. The limit of detection and limit of quantification were 0.0002 mg/mL and 0.0005 mg/mL, respectively. The linearity calibration curve of (R)-2-aminobutanamide was shown good from the range of 0.0005 mg/mL to 0.004 mg/mL. The recovery of (R)-2-aminobutanamide isomer was between the range of 93 to 106 % in presence of (S)-2-aminobutanamide. The method was validated and found to be precise, accurate and robust. The method can be used for determination of (R)-2-aminobutanamide in presence of (S)-2-aminobutanamide, which is the key intermediate for preparation of levetiracetam. This method was validated in as per ICH Q2 (R1) and USP validation of compendial methods (1225).

Development and Validation of a Reversed-Phase Chiral HPLC Method to Determine the Chiral Purity of Bulk Batches of (S)-Enantiomer in Afoxolaner

2017 ◽  
Vol 100 (1) ◽  
pp. 65-73
Author(s):  
Nilusha Padivitage ◽  
Satish Kumar ◽  
Abu Rustum
Keyword(s):  
Method Development ◽  
Specific Rotation ◽  
Reversed Phase ◽  
Hplc Method ◽  
Racemic Mixture ◽  
Chiral Hplc ◽  
Development Tool ◽  
Chiral Purity ◽  
Development And Validation ◽  
First Time

Abstract Afoxolaner is a new antiparasitic molecule from the isoxazoline family that acts on insect acarine g-aminobutyric acid and glutamate receptors. Afoxolaner is a racemic mixture, which has a chiral center at the isoxazoline ring. A reversed-phase chiral HPLC method has been developed to determine the chiral purity of bulk batches of (S)-enantiomer in afoxolaner for the first time. This method can also be used to verifythat afoxolaner is a racemic mixture, which was demonstrated by specific rotation. ChromSword, an artificial intelligence method development tool, was used for initial method development. The column selected for the final method was CHIRALPAK AD-RH (150 × 4.6 mm, 5 μm particle size), maintained at 45°C, and isocratic elution using water–isopropanol–acetonitrile (40 + 50 + 10, v/v/v) as the mobile phasewith a detection wavelength of 312 nm. The run time for the method was 11 min. The resolution and selectivity factors of the two enantiomers were 2.3 and 1.24, respectively. LOQ and LOD of the method were 1.6 and 0.8 μg/mL, respectively. This method was appropriately validated according to International Conference on Harmonization guidelines for its intended use.

A Validated Chiral HPLC Method for the Determination of Enantiomeric Purity of R-β-amino-β-(4-methoxyphenyl) Propionic Acid

2006 ◽  
Vol 65 (1-2) ◽  
pp. 81-84 ◽  
Author(s):  
P. Madhavan ◽  
B. M. Rao ◽  
Pravin ◽  
Abhishek ◽  
P. R. Kumar ◽  
...  
Keyword(s):  
Propionic Acid ◽  
Hplc Method ◽  
Enantiomeric Purity ◽  
Chiral Hplc
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