A validated chiral HPLC method for the enantiomeric separation of tolterodine tartarate

2004 ◽  
Vol 35 (5) ◽  
pp. 1279-1285 ◽  
Author(s):  
Y.Ravindra Kumar ◽  
G. Ramulu ◽  
V.V. Vevakanand ◽  
Gopal Vaidyanathan ◽  
Keesari srinivas ◽  
...  
Keyword(s):  
Enantiomeric Separation ◽  
Hplc Method ◽  
Chiral Hplc

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)

A Validated Chiral HPLC Method for the Enantiomeric separation of Mefloquine

2019 ◽  
Vol 12 (5) ◽  
pp. 2304
Author(s):  
S. Jenifer Ashwini ◽  
S. T. Narenderan ◽  
S. N. Meyyanathan ◽  
B. Babu ◽  
B. Gowramma
Keyword(s):  
Enantiomeric Separation ◽  
Hplc Method ◽  
Chiral Hplc

A Validated Chiral HPLC Method for the Enantiomeric Separation of Melphalan HCl

2013 ◽  
Vol 781-784 ◽  
pp. 993-998
Author(s):  
Li Ping Gao ◽  
Wen Juan Li ◽  
Xin Ping Wang
Keyword(s):  
Perchloric Acid ◽  
Mobile Phase ◽  
Enantiomeric Separation ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Hplc Separation ◽  
Perchloric Acid Solution ◽  
Anti Cancer ◽  
Chromatographic Resolution

A new and accurate chiral HPLC method was developed for the determination of Melphalan HCl, L-Phenylalanine, 4-bis (2-chloroethyl) amino hydrochloride an anti-cancer chemotherapy drug and its potential impurity namely D-Phenylalanine, 4-bis (2-chloroethyl) amino hydrochloride ( D-enantiomer) in bulk substance. HPLC separation was carried out by reverse phase chromatography on Crownpak CR (+) (5μm, 4.0x150mm) with a mobile phase composed of perchloric acid (pH 4.0): methanol in the ratio of 90:10. Melphalan and its potential impurities were baseline resolved in the optimized method. The pH of perchloric acid solution in the mobile phase has played a key role in achieving chromatographic resolution between the enantiomers and in enhancing chromatographic efficiency. The developed method was completely validated and proved to be robust. The validated method yielded good results regarding specificity, precision, linearity, accuracy, robustness, sensitivity. Melphalan HCl sample solution is found to be stable for at least 60hrs at room temperature. The proposed method was found to be suitable and accurate for quantitative determination of Melphalan HCl and its D-enantiomer in bulk substance.

scholarly journals Enantiomeric Determination of Carvedilol by a Newly Developed and Validated Chiral HPLC Method

2019 ◽  
Vol 18 (1) ◽  
pp. 61-68
Author(s):  
Asma Rahman ◽  
Mohammad Rashedul Haque ◽  
Md Zakir Sultan ◽  
M Muhibur Rahman ◽  
Mohammad A Rashid
Keyword(s):  
Isopropyl Alcohol ◽  
Stationary Phases ◽  
Enantiomeric Separation ◽  
Hplc Method ◽  
Regression Coefficients ◽  
Chiral Hplc ◽  
Pharmaceutical Dosage Forms ◽  
Average Percentage ◽  
Quantitation Limit

A new simple, selective, linear and accurate chiral HPLC method for assay of carvedilol enantiomers was developed with immobilized cellulose chiral stationary phases under normal-phase mode using hexane: isopropyl alcohol: diethyl amine: acetic acid (40: 60: 0.7: 0.3, v/v) as the mobile phase at a flow rate of 1.0 mL/min and detection at 220 nm. The method was validated for linearity, precision, accuracy, ruggedness, robustness and stability as per the guidelines of USP and ICH. The regression coefficients (r2) of the linearity were found to be 0.999 for both S- and R- carvedilol, detection limit (LOD) were 1.67 and 1.78 μg/mL and quantitation limit were also found to be 5.06 and 5.41 μg/mL for S- and R- carvedilol, respectively. The average percentage of recovery was found to be 99.59% to 100.83% for S- and 98.42% to 100.18% for R- carvedilol, respectively. The new method can be used for enantiomeric separation and estimation of carvedilol in pharmaceutical dosage forms without any interference. Dhaka Univ. J. Pharm. Sci. 18(1): 61-68, 2019 (June)

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

Rapid Enantiomeric Separation and Quantitation of Levetiracetam on α-Acid Glycoprotein (AGP) Chiral Stationary Phase by High-Performance Liquid Chromatography

2015 ◽  
Vol 98 (6) ◽  
pp. 1529-1534 ◽  
Author(s):  
Rouhollah Heydari ◽  
Mojtaba Shamsipur
Keyword(s):  
High Performance Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Chiral Stationary Phase ◽  
Bulk Material ◽  
Enantiomeric Separation ◽  
Hplc Method ◽  
Chiral Hplc ◽  
Uv Detector ◽  
Acid Glycoprotein

Abstract A new, simple, and rapid chiral HPLC method was developed for enantioselective analysis of levetiracetam and its enantiomer [(R )-α-ethyl-2- oxo-pyrrolidine acetamide] in a pharmaceutical formulation and bulk material. Enantiomeric separation was achieved on a chiral-α1 -acid glycoprotein (AGP) column (150 × 4.0 mm, 5 μm) using an isocratic mobile phase of phosphate buffer (pH = 7) at a flow rate of 0.7 mL/min. The UV detector was set at 210 nm. Calibration curves were linear in the range of 1–100 μg/mL and 0.4–20 μg/mL for levetiracetam and the (R)-enantiomer, respectively. LOD and LOQ for the (R)-enantiomer were 0.1 and 0.4 μg/mL, respectively. The run time of analysis was less than 5.0 min.

scholarly journals Enantiomeric separation of Midodrine hydrochloride in bulk and pharma-ceutical dosage form by chiral HPLC

2019 ◽  
Vol 10 (3) ◽  
pp. 1608-1611
Author(s):  
Jenifer Ashwini S ◽  
Narenderan ST ◽  
Meyyanathan SN ◽  
Babu B ◽  
Gowramma B
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Enantiomeric Separation ◽  
Hplc Method ◽  
Ammonium Bicarbonate ◽  
Chiral Hplc ◽  
Column Temperature ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

A simple, sensitive chiral liquid chromatographic method was developed for the separation and quantification of enantiomers Midodrine. A chiral PAK IG-3 (150 x 4.6 mm) 3µm column was used for the separation of the enantiomers. The mobile phase consists of 10 mM ammonium bicarbonate in water and acetonitrile in the ratio of 95:5, v/v with a flow rate of 0.7 ml/min. The detection was done at 290 nm with column temperature maintained at 40°C. The method linear ranged between 10 – 110 μg/ml and 5 – 100 μg/ml for (+) and (-) Midodrine enantiomers.  The recovery of the method was found to be in the range of 99.1 to 101.2 %. The detection limit for the (+) and (-) enantiomers was found to be 4 μg/ml and 1 μg/ml, respectively. A simple validated chiral HPLC method with reverse elusion is described for the separation and quantification of the enantiomers of Midodrine in bulk and formulation.

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.

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).

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