Development and validation of HPLC method for enantioseparation of Ibrutinib on immobilized chiral stationary phase

2021 ◽  
Author(s):  
Raman Reddy Gopireddy ◽  
Arthanareeswari Maruthapillai ◽  
Sudarshan Mahapatra ◽  
M. Tamilselvi
Keyword(s):  
Stationary Phase ◽  
Chiral Stationary Phase ◽  
Hplc Method ◽  
Development And Validation

Development and Validation of Teneligliptin Stereoisomers by HPLC Using Cellulose Based Immobilized Polysaccharide Chiral Stationary Phase

2020 ◽  
Vol 17 ◽  
Author(s):  
Gunnam Srinivasu ◽  
Ch Thirupathia ◽  
Ch Lakshmi Narayanaa ◽  
Ch Parameswara Murthy ◽  
Sarah Imam Siddiqui
Keyword(s):  
Stationary Phase ◽  
High Performance ◽  
Chiral Stationary Phase ◽  
Limit Of Detection ◽  
Research Work ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Bulk Drug ◽  
Development And Validation ◽  
Isocratic Mode

Background:: There is no single chiral method for the quantitation of teneligliptin stereoisomers by high performance liquid chromatography (HPLC). Hence, there is a need for the quantification of teneligliptin (TNGP) and its stereoisomers. Objective:: The main aim of the research work is to develop a novel simple, selective, precise and accurate HPLC method for separation of TNGP and its stereoisomers. Methods:: Different screening trials were executed by changing the mobile phase compositions to normal phase and polar mode and also by utilizing the different immobilized polysaccharide chiral columns like CHIRALPAK IA, IC, ID, IE, IF and IG. All the stereoisomers were eluted with high resolution, on CHIRALPAK IC-3 (4.6×250 mm), 3 μm chiral stationary phase (CSP) with flow rate of 0.7 mL/min. The chromatographic system was processed with isocratic mode comprising ethanol: acetonitrile: ethanolamine in the proportion of 90:10:0.1% v/v/v with column oven temperature of 15 °C and detection wavelength of 250 nm. Results:: The limit of detection (LOD) and limit of quantification (LOQ) values of TNGP(API), R,S-isomer, S,R-isomer and R,R-isomer were found to be 0.036/0.11, 0.029/0.09, 0.038/0.011 and 0.020/0.06 μg/mL, respectively. The method was found to be precise, accurate and linear (R2 > 0.999). Conclusion:: The developed method also successfully applied for the quantification of bulk drug without any interference with the extraneous components. Hence, the method can be utilized successfully in the pharmaceutical organizations for the separation and quantification of TNGP isomers.

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 Direct Stereoselective Method Development and Validation of Elagolix on Zwitterionic Chiral Stationary Phase by High-Pressure Liquid Chromatography

2020 ◽  
pp. 517-524
Author(s):  
Thirupathi Choppari ◽  
Srinivasu Gunnam ◽  
Lakshmi Narayana Chennuru ◽  
Parameswara Murthy Cherla
Keyword(s):  
Stationary Phase ◽  
Chiral Stationary Phase ◽  
Method Development ◽  
Drug Product ◽  
Research Work ◽  
Cinchona Alkaloid ◽  
Chromatographic Technique ◽  
Ich Guidelines ◽  
Development And Validation ◽  
High Degree

A specific, sensitive and accurate chiral technique has been developed for the quantification of elagolix enantiomer in a drug product. The present research work represents the development and validation of chromatographic technique for the separation of elagolix enantiomers on a chiral stationary phase (CSP) comprising a zwitterionic selector derived from cinchona alkaloid and sulfonic acid CHIRALPAK ZWIX (+)  under isocratic condition containing 50mM Acetic acid and 25mM diethyl amine in water and methanol in the ratio of 02:98 v/v with 0.5 ml min-1 flow rate. Temperature of the column was monitored at 40°C with a resolving factor more than 3.2. The eluted compounds were monitored at 275 nm. The optimized method has high degree of selectivity with lower limiting values of detection and quantitation and were found to be 2.0 ng/ml and 7.5 ng/ml, respectively for the enantiomeric chiral impurity. The developed method was subjected for validation as per the ICH guidelines, produced good findings regarding specificity, accuracy, precision, robustness and linearity.

Development and validation of a fast HPLC method for methyldopa enantiomers using superficially porous particle based macrocyclic glycopeptide stationary phase

2021 ◽  
Vol 164 ◽  
pp. 105957
Author(s):  
Mariana da Silva Gonçalves ◽  
Daniel W. Armstrong ◽  
Lucio Mendes Cabral ◽  
Eduardo Costa Pinto ◽  
Valeria Pereira de Sousa
Keyword(s):  
Stationary Phase ◽  
Hplc Method ◽  
Porous Particle ◽  
Macrocyclic Glycopeptide ◽  
Development And Validation

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.

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