Improving the Current European Pharmacopoeia Enantio-Selective HPLC Method for the Determination of Enantiomeric Purity in Atorvastatin Calcium Salt Drug Substance
Abstract
1. Introduction
2. Materials and Methods
2.1. Chemicals and Reagents
2.2. Instruments
2.3. HPLC Operating Conditions and Partial Method Validation
3. Results
3.1. Enantioseparation under Normal-Phase Conditions
3.2. Chemo- and Diastereo-Selectivity of the Normal-Phase Enantio-Selective Method
3.3. Optimization of the Normal-Phase Enantio-Selective EP Method
3.4. Influence of Ethanol Percentage on Elution Order of Impurities E and H
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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CSP | Mobile Phase | k1 | k2 | α | Rs |
---|---|---|---|---|---|
Chiralpak IA-3 | n-Hexane-EtOH-TFA (90:10:0.1) | 2.52 | 3.10 | 1.23 | 2.62 |
n-Hexane-IPA-TFA (90:10:0.1) | 3.70 | - | 1.00 | - | |
Chiralpak AD-3 | n-Hexane-EtOH-TFA (90:10:0.1) | 4.11 | 7.36 | 1.79 | 4.10 |
n-Hexane-EtOH-TFA (80:20:0.1) | 0.72 | 1.27 | 1.75 | 1.99 | |
n-Hexane-IPA-TFA (90:10:0.1) | 5.98 | - | 1.00 | - | |
Chiralpak ID-3 | n-Hexane-EtOH-TFA (90:10:0.1) | 3.57 | - | 1.06 | - |
n-Hexane-IPA-TFA (90:10:0.1) | 7.14 | - | 1.06 | - | |
Chiralpak IG-3 | n-Hexane-EtOH-TFA (90:10:0.1) | 4.87 | 5.49 | 1.13 | 1.20 |
n-Hexane-IPA-TFA (90:10:0.1) | 11.1 | - | 1.00 | - | |
Chiralpak IH-3 | n-Hexane-EtOH-TFA (90:10:0.1) | 2.89 | - | 1.00 | - |
n-Hexane-IPA-TFA (90:10:0.1) | 4.13 | - | 1.00 | - |
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Mammone, F.R.; Sadutto, D.; D’Ettorre, G.; Mosca, A.; Cirilli, R. Improving the Current European Pharmacopoeia Enantio-Selective HPLC Method for the Determination of Enantiomeric Purity in Atorvastatin Calcium Salt Drug Substance. Separations 2024, 11, 154. https://doi.org/10.3390/separations11050154
Mammone FR, Sadutto D, D’Ettorre G, Mosca A, Cirilli R. Improving the Current European Pharmacopoeia Enantio-Selective HPLC Method for the Determination of Enantiomeric Purity in Atorvastatin Calcium Salt Drug Substance. Separations. 2024; 11(5):154. https://doi.org/10.3390/separations11050154
Chicago/Turabian StyleMammone, Francesca Romana, Daniele Sadutto, Giulia D’Ettorre, Antonina Mosca, and Roberto Cirilli. 2024. "Improving the Current European Pharmacopoeia Enantio-Selective HPLC Method for the Determination of Enantiomeric Purity in Atorvastatin Calcium Salt Drug Substance" Separations 11, no. 5: 154. https://doi.org/10.3390/separations11050154
APA StyleMammone, F. R., Sadutto, D., D’Ettorre, G., Mosca, A., & Cirilli, R. (2024). Improving the Current European Pharmacopoeia Enantio-Selective HPLC Method for the Determination of Enantiomeric Purity in Atorvastatin Calcium Salt Drug Substance. Separations, 11(5), 154. https://doi.org/10.3390/separations11050154