Determination of AR-42 enantiomeric purity by HPLC on chiral stationary phase

Determination of AR-42 enantiomeric purity by HPLC on chiral stationary phase A sensitive and accurate liquid chromatographic method for the determination of AR-42 enantiomeric purity has been developed and validated. Baseline separation with a resolution higher than 1.9 was accomplished within 10 min using a CHIRALPAK AD column (250 mm × 4.6 mm; particle size 5 μm) and n-hexane/2-propanol/diethylamine (75:25:0.1 v/v/v) as mobile phase at a flow rate of 1 mL min−1. Eluted analytes were monitored by UV absorption at 260 nm. The effects of mobile phase components, temperature and flow rate on enantiomeric selectivity and resolution of enantiomers were investigated. Calibration curves were plotted within the concentration range between 0.001 and 0.5 mg mL−1 (n = 10), and the recoveries between 98.23 and 101.87% were obtained, with relative standard deviation lower than 1.31%. Limit of detection and limit of quantitation for AR-42 were 0.39 and 1.28 μg mL−1 and for its enantiomer were 0.36 and 1.19 μg mL−1, respectively. It was demonstrated that the developed method was accurate, robust and sensitive for the determination of enantiomeric purity of AR-42, especially for the analysis of bulk samples. http://www.deepdyve.com/assets/images/DeepDyve-Logo-lg.png Journal of the Iranian Chemical Society Springer Journals

Determination of AR-42 enantiomeric purity by HPLC on chiral stationary phase

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Publisher
Springer Berlin Heidelberg
Copyright
Copyright © 2017 by Iranian Chemical Society
Subject
Chemistry; Analytical Chemistry; Inorganic Chemistry; Physical Chemistry; Biochemistry, general; Organic Chemistry
ISSN
1735-207X
eISSN
1735-2428
D.O.I.
10.1007/s13738-017-1130-0
Publisher site
See Article on Publisher Site

Abstract

A sensitive and accurate liquid chromatographic method for the determination of AR-42 enantiomeric purity has been developed and validated. Baseline separation with a resolution higher than 1.9 was accomplished within 10 min using a CHIRALPAK AD column (250 mm × 4.6 mm; particle size 5 μm) and n-hexane/2-propanol/diethylamine (75:25:0.1 v/v/v) as mobile phase at a flow rate of 1 mL min−1. Eluted analytes were monitored by UV absorption at 260 nm. The effects of mobile phase components, temperature and flow rate on enantiomeric selectivity and resolution of enantiomers were investigated. Calibration curves were plotted within the concentration range between 0.001 and 0.5 mg mL−1 (n = 10), and the recoveries between 98.23 and 101.87% were obtained, with relative standard deviation lower than 1.31%. Limit of detection and limit of quantitation for AR-42 were 0.39 and 1.28 μg mL−1 and for its enantiomer were 0.36 and 1.19 μg mL−1, respectively. It was demonstrated that the developed method was accurate, robust and sensitive for the determination of enantiomeric purity of AR-42, especially for the analysis of bulk samples.

Journal

Journal of the Iranian Chemical SocietySpringer Journals

Published: May 15, 2017

References

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