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

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

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.

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 HPLC/UV-Spectrophotometric Procedures for Metronidazole Quantitative Determination

2018 ◽  
Vol 9 (3) ◽  
Author(s):  
Klimenko Lina Yu ◽  
Shkarlat Galyna L ◽  
Shovkova Zoia V ◽  
Yaremenko Vitaliy D ◽  
Shpychak Oleg S
Keyword(s):  
Quantitative Determination ◽  
Sodium Hydroxide Solution ◽  
Gradient Elution ◽  
Calibration Model ◽  
Column Temperature ◽  
Medical Laboratories ◽  
Accuracy And Precision ◽  
Development And Validation ◽  
Gradient Elution Mode ◽  
Potential Object

Metronidazole is the most popular representative of antiprotozoal medicines from the group of 5-nitroimidazoles. Metronidazole blocks the enzymes of alcohol dehydrogenase and acetaldehyde dehydrogenase, therefore when its joint taking with alcohol it is observed the strong intoxication syndrome and fatal poisonings too. Therefore metronidazole can be a potential object of chemical toxicological investigations. The purpose of our paper is to develop HPLC/UV-procedure of metronidazole quantification with application of the system of HPLC-analyzer MiLiChrome® A-0230 implemented in practice of forensic medical laboratories in Russia and Ukraine and carry out step-by-step validation of the developed procedure. Chromatographic conditions: Eluent A (0.2 M LiClO4 – 0.005 M HClO4) and Eluent B (acetonitrile) wereused as the mobile phase components; HPLC microcolumn Ø2×75 mm and ProntoSIL 120-5-C18 AQ, 5 μm were used as an analytical column; temperature was 40°С; flow rate was 100 μl/min; gradient elution mode was from 5% to 100% Eluent B for 40 min, then 100% Eluent B for 3 min; detection was performed at 277 nm. Retention time for metronidazole is 5.95 min. Since metronidazole is easy soluble and stable enough in the solutions of diluted alkalis 0.001 M sodium hydroxide solution has been proposed for preparation of the solutions in developing HPLC/UV-procedure of metronidazole quantification. Validation of the procedure has been carried out in the variants of the method of calibration curve and method of standard by such parameters as in process stability, linearity/calibration model, accuracy and precision within 3 different analytical runs using different batches of reagents and different glassware; experiments have been performed by three different analysts. New procedure of metronidazole quantitative determination by the method of HPLC/UV has been developed. Its validation has been carried out and acceptability for application has been shown.

LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT AND VALIDATION OF RELATED IMPURITIES OF LURASIDONE AND ITS FORMULATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (09) ◽  
pp. 41-48
Author(s):  
R. N Kachave ◽  
◽  
P. B. Mandlik ◽  
S. R. Nisal
Keyword(s):  
Method Development ◽  
Gradient Elution ◽  
Hplc Method ◽  
Chromatography Method ◽  
Related Impurities ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Liquid Chromatography Method ◽  
The Stability ◽  
Development And Validation

An RP-HPLC method was developed for the quantification of related impurities of lurasidone and its formulation. The chromatographic separation employs gradient elution using an Inertsil ODS C18 (150x4.6) mm, 5μm columns. Mobile phase consisting of solvent A-buffer (pH 3.0): methanol (90:10 %v/v) and solvent B-acetonitrile: water (80:20 % v/v) delivered at a flow rate of 1.0 mL/min. The analytes were detected and quantified at 210 nm using PDA. The method was validated as per ICH guidelines, demonstrating to be a simple, precise, selective, linear and accurate within the corresponding range of impurities of lurasidone. Linearity was observed in the concentration range of 2-6 µg/mL. The RT for Lurasidone was about 18.5 min and three known impurities at RRT about 0.15, 0.21 and 0.36. The specificity of the method was investigated under different stress conditions including hydrolytic, oxidative, photolytic and thermal as recommended by ICH guidelines. Relevant degradation was found to take place under oxidative conditions. Degradation impurities did not interfere with the RT of drug. The peak purity obtained with the aid of PDA detection and satisfactory resolution between related impurities established the specificity of the determination. All these results provide the stability indicating capability of the method.

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.

scholarly journals HPLC Estimation of New Impurity Methyl Ezetimibe in Ezetimibe Drug

2020 ◽  
Vol 32 (6) ◽  
pp. 1309-1313
Author(s):  
Duggirala Parvatha Venkata Vardhani Devi ◽  
Kapavarapu Maruthi Venkata Narayanarao ◽  
Pulipaka Shyamala ◽  
Rallabhandi Murali Krishna ◽  
Komali Siva Prasad
Keyword(s):  
Limit Of Detection ◽  
Signal To Noise Ratio ◽  
Gradient Elution ◽  
Hplc Method ◽  
The Novel ◽  
Signal To Noise ◽  
Drug Substances ◽  
Chromatographic Detection ◽  
Noise Ratio ◽  
Gradient Elution Mode

A new gradient elution mode HPLC method was developed and validated to detect and monitor the novel impurity namely methyl ezitimibe in ezetimibe drug substances. Chromatographic detection and analysis of methyl ezetimibe was performed on XBridge C18 column with mobile phase consisting of 0.02 M phosphate buffer (pH 5) and acetonitrile with 1 mL/min flow rate in gradient elution mode. Methyl ezetimibe was detected and monitored at 248 nm. The calibration curve was linear over range of 0.015 to 0.219% concentration. The limit of detection and quantification were computed as 0.005% (signal to noise ratio 3.60) and 0.015% (signal to noise ratio 15.96), respectively. The precision was 0.97% (%RSD) and accuracy was 93.2 to 98.2% (recovery). The developed method was proved suitable to detect and monitor methyl ezetimibe impurity in ezetimibe drug substances.

scholarly journals Development and Validation of RP-Chiral HPLC Method for Determination of (R)-Enantiomer Excess Content in Efavirenz

2020 ◽  
Vol 32 (9) ◽  
pp. 2208-2212
Author(s):  
CH. RAMESH ◽  
DHARMASOTH RAMA DEVI DEVI ◽  
M.N.B. SRINIVAS ◽  
S. RADHA KRISHNA ◽  
NAGARAJU RAJANA ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Enantiomer Excess ◽  
Development And Validation ◽  
Methyl Phenyl

simple, specific, linear, accurate and precise reverse phase chiral HPLC method was developed for the separation of efavirenz enantiomers by using the Lux Amylose-2 column containing amylose tris(5-chloro-2-methyl phenyl carbamate) as a stationary phase. The mobile phase consists of 0.1 % formic acid in water and acetonitrile (55:45, v/v). The flow rate was kept at 1.0 mL/min and the detection wavelength used 252 nm and the column temperature was set at 25 ºC. The limit of detection was 0.01 mg/mL and the limit of quantification was 0.04 mg/mL. The linearity calibration curve of (R)-enantiomer was shown well from the range of 0.04 mg/mL to 0.4 mg/mL. The values of the correlation coefficient were 0.999 and 0.999 for (R)-enantiomer and (S)-efavirenz, respectively. The percentage recoveries of (R)-enantiomer from efavirenz drug substance were ranged from 93.5% to 107.5%. The results demonstrated that developed RP-chiral HPLC method was simple, precise, robust and applicable for the estimation of (R)-enantiomer in efavirenz API. This method was validated in as per ICH Q2 (R1) and USP validation of compendial methods <1225>.

scholarly journals Development and Validation of a Chiral HPLC Method for Quantitative Analysis of Enantiomeric Escitalopram

2018 ◽  
Vol 16 (2) ◽  
pp. 165-172 ◽  
Author(s):  
Asma Rahman ◽  
Mohammad Rashedul Haque ◽  
M Muhibur Rahman ◽  
Mohammad A Rashid
Keyword(s):  
Pharmaceutical Preparations ◽  
Enantiomeric Separation ◽  
Hplc Method ◽  
Enantiomeric Purity ◽  
Chiral Hplc ◽  
Average Percentage ◽  
Quantitation Limit ◽  
Relative Standard ◽  
Development And Validation

In the present study a rapid, accurate and precise chiral HPLC method was developed and validated for enantiomeric separation of racemate citalopram and escitalopram according to the guidelines of United States of Pharmacopeia (USP) and International Conference on Harmonization (ICH). The chiral chromatographic separation was achieved with ammonium acetate/ ethanol/ 2-propanol/ methylene dichloride (100 : 150 : 70 : 30, v/v) at a flow rate of 0.5 ml/min using a chiral CD-PH column. The HPLC analyses were monitored at 254 nm. The method showed a good linearity with regression coefficient (r2) of 0.998 in the range of 20.0-70.0 μg/ml for escitalopram. The detection limit (LOD), quantitation limit (LOQ) and average percentage of recovery for escitalopram were found to be 2.54, 7.68 μg/ml and 100.28% to 102.86%, respectively. The percentage of relative standard deviation (%RSD) for intra- and inter- day precision were found as 0.16% and 0.09%, respectively. The established method proved as reproducible with a %RSD value of less than 2 and having the robustness within specified limit. The present study also showed the enantiomeric purity or excess (%ee) of seven pharmaceutical preparations of escitalopram. Thus the proposed chiral method can be applied for the enantiomeric purity determination of escitalopram formulations.Dhaka Univ. J. Pharm. Sci. 16(2): 165-172, 2017 (December)

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