Insights into the Mechanism of Separation of Bisphosphonates by Zwitterionic Hydrophilic Interaction Liquid Chromatography: Application to the Quantitation of Risedronate in Pharmaceuticals
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemicals and Reagents
2.2. Instrumentation
2.3. Statistical Analysis
2.4. Stock and Working Standard Solutions
2.5. Assay Procedure for the Pharmaceutical Samples
2.6. Accelerated and Long-Term Stability Studies
3. Results and Discussion
3.1. Method Development
3.1.1. Effect of Chromatographic Parameters on the Bisphosphonates Retention
3.1.2. Optimization of the Chromatographic Parameters for the Quantitation of Risedronate
3.2. Method Validation
3.2.1. Selectivity
3.2.2. Statistical Analysis of Data
3.2.3. Accelerated and Long-Term Stability Studies
3.3. Analysis of Commercial Tablets
4. Conclusions
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Concentration Range, μg mL−1 | Regression Equations a | r b | Standard Deviation | Sr c | |
---|---|---|---|---|---|
Slope | Intercept | ||||
Mean of 3 calibration curves over a period of 1 month | |||||
1.5–5 | SRsd = 3.029 × CRsd + 1.76 | ≥0.9991 | 1.7 × 10−3 | 3.2 × 10−2 | ≤0.24 |
Risedronate | Concentration (μg mL−1) | ||
---|---|---|---|
Added concentration | 1.5 | 3.5 | 5 |
Run 1 (mean ± SD) | 1.4669 ± 0.0051 | 3.556 ± 0.022 | 5.013 ± 0.046 |
Run 2 (mean ± SD) | 1.4589 ± 0.0033 | 3.567 ± 0.012 | 5.022 ± 0.088 |
Run 3 (mean ± SD) | 1.4715 ± 0.0044 | 3.5628 ± 0.0091 | 4.973 ± 0.012 |
Overall mean | 1.4658 | 3.5618 | 5.0031 |
Intra-day CV(%) a | 0.3 | 0.5 | 0.6 |
Inter-day CV(%) a | 0.5 | 0.05 | 0.6 |
Overall accuracy Er% b | −2.3 | 1.8 | 0.1 |
Degradation Conditions/Time | Time | Concentration (μg mL−1) (Mean ± S.D., n = 3) | % Recovery (Mean ± S.D., n = 3) | Degradation Products Retention Time (min) |
1.0 M HCl, 50 °C | 1 day | 3.467 ± 0.038 | 99.0 ± 1.1 | - |
2 days | 3.469 ± 0.041 | 99.1 ± 1.2 | - | |
8 days | 3.036 ± 0.040 | 86.7 ± 1.1 | <3 | |
10 days | 2.736 ± 0.032 | 78.1 ± 0.9 | <3 | |
1.0 M NaOH, 25 °C | 1 day | 2.757 ± 0.073 | 78.8 ± 2.1 | <3 |
3 % v/v H2O2, 25 °C | 1 h | 3.211 ± 0.042 | 91.7 ± 1.2 | - |
2 h | 3.094 ± 0.041 | 88.4 ± 1.1 | <3 | |
3 h | 2.895 ± 0.047 | 82.7 ± 1.4 | <3 | |
Long-Term Stability Studies | Time | Amount (mg) Per Tablet (Mean ± S.D., n = 3) | % Recovery (Mean ± S.D., n = 3) | Degradation Products Retention Time (min) |
50 ± 2 °C 15% humidity | 1 month | 32.79 ± 0.51 | 100.9 ± 1.5 | - |
3 months | 32.41 ± 0.46 | 99.7 ± 1.3 | - | |
50 ± 2 °C 75% humidity | 1 month | 32.38 ± 0.44 | 99.6 ± 1.2 | - |
3 months | 25.22 ± 0.63 | 77.6 ± 1.8 | <3 |
Test | Amount (mg) Per Tablet (Mean ± SD, n = 10) | % Recovery (Mean ± SD, n = 10) |
---|---|---|
Quality control | 32.3 ± 0.2 | 99.3 ± 0.7 |
Content uniformity | 32.6 ± 0.4 | 100.2 ± 1.2 |
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Panderi, I.; Taxiarchi, E.; Pistos, C.; Kalogria, E.; Vonaparti, A. Insights into the Mechanism of Separation of Bisphosphonates by Zwitterionic Hydrophilic Interaction Liquid Chromatography: Application to the Quantitation of Risedronate in Pharmaceuticals. Separations 2019, 6, 6. https://doi.org/10.3390/separations6010006
Panderi I, Taxiarchi E, Pistos C, Kalogria E, Vonaparti A. Insights into the Mechanism of Separation of Bisphosphonates by Zwitterionic Hydrophilic Interaction Liquid Chromatography: Application to the Quantitation of Risedronate in Pharmaceuticals. Separations. 2019; 6(1):6. https://doi.org/10.3390/separations6010006
Chicago/Turabian StylePanderi, Irene, Eugenia Taxiarchi, Constantinos Pistos, Eleni Kalogria, and Ariadni Vonaparti. 2019. "Insights into the Mechanism of Separation of Bisphosphonates by Zwitterionic Hydrophilic Interaction Liquid Chromatography: Application to the Quantitation of Risedronate in Pharmaceuticals" Separations 6, no. 1: 6. https://doi.org/10.3390/separations6010006