Development and Validation of Stability-Indicating Assay Method for a Novel Oxazolidinone (PH-192) with Anticonvulsant Activity by Using UHPLC-QToF-MS
Abstract
:1. Introduction
2. Results and Discussion
2.1. Method Validation
2.1.1. Linearity and Sensitivity
2.1.2. Precision and Accuracy
2.1.3. Evaluation of PH-192 Extraction and Stability in Human Plasma
2.1.4. Stability Study
3. Materials and Methods
3.1. Chemicals
3.2. Solutions
3.3. Human Plasma Extraction Procedure
3.4. Instrumentation
3.4.1. Ultra-Pressure Liquid Chromatography
3.4.2. Liquid Chromatography-Mass Spectrometry
3.4.3. Calibration Procedure for Mass Spectrometry
3.5. Method Validation
3.5.1. Calibration Curve
3.5.2. Accuracy and Precision
3.5.3. Extraction Recovery and Matrix Effect
3.5.4. Evaluation of PH-192 Extraction and Stability in Human Plasma
3.5.5. Limit of Detection (LOD) and Limit of Quantification (LOQ)
3.6. Forced Degradation Studies
3.6.1. Acidic Degradation
3.6.2. Basic Degradation
3.6.3. Oxidation Degradation
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Sample Availability
References
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Parameters | PH-192 |
---|---|
Range µg/mL | 1–80 |
Regression Equation | y = 0.0867x − 0.0403 |
Correlation coefficient (r) | 0.9998 |
LOQ (µg/mL) | 1 |
LOD (µg/mL) | 0.33 |
Intra-assay precision b | 5.8 |
Inter-assay precision b | 7.4 |
Accuracy c | 96.66% |
Precision | PH-192 Concentration μg/mL | Mean ± SD (n = 3) Observed/μg/mL | Precision a (%) | Accuracy b (%) |
---|---|---|---|---|
Intra-Assay Precision And Accuracy Data for PH-192 Determination in Bulk Powder Using UPLC-UV. | 1 | 0.966 ± 0.056 | 5.8 | 96.66 |
20 | 19.91 ± 0.158 | 0.8 | 99.55 | |
80 | 79.96 ± 0.165 | 0.2 | 99.96 | |
Inter-Assay Precision And Accuracy Data for PH-192 Determination in Bulk Powder Using UPLC-UV. | 1 | 0.943 ± 0.070 | 7.4 | 94.33 |
20 | 19.77 ± 0.305 | 1.5 | 98.85 | |
80 | 79.27 ± 0.409 | 0.5 | 99.08 |
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Al-Tannak, N.F.; Phillips, O.A.; Kamal, H.J.; Hemdan, A. Development and Validation of Stability-Indicating Assay Method for a Novel Oxazolidinone (PH-192) with Anticonvulsant Activity by Using UHPLC-QToF-MS. Molecules 2022, 27, 1090. https://doi.org/10.3390/molecules27031090
Al-Tannak NF, Phillips OA, Kamal HJ, Hemdan A. Development and Validation of Stability-Indicating Assay Method for a Novel Oxazolidinone (PH-192) with Anticonvulsant Activity by Using UHPLC-QToF-MS. Molecules. 2022; 27(3):1090. https://doi.org/10.3390/molecules27031090
Chicago/Turabian StyleAl-Tannak, Naser F., Oludotun A. Phillips, Husein J. Kamal, and Ahmed Hemdan. 2022. "Development and Validation of Stability-Indicating Assay Method for a Novel Oxazolidinone (PH-192) with Anticonvulsant Activity by Using UHPLC-QToF-MS" Molecules 27, no. 3: 1090. https://doi.org/10.3390/molecules27031090