Optimization of Chromatographic Conditions with QbD for Method Development and Validation of Bosutinib by HPLC: Applications in Dosage Forms and Rat Plasma Analysis
Abstract
:1. Introduction
2. Experimental Work
2.1. Materials
2.2. Instruments/Apparatus
2.3. Methods
2.3.1. Risk Assessment Studies
2.3.2. Optimization
2.3.3. Method Development
2.3.4. Stock, Standard, and Quality-Control Sample
2.3.5. Preparation of Calibration Curve
2.3.6. Preparation of Tablet Formulation Solution
2.3.7. Preparation of Rat Plasma Samples
2.4. Method Validation
2.4.1. System Suitability Test
2.4.2. Linearity
2.4.3. Precision and Accuracy
2.4.4. Solution Stability
2.4.5. Robustness Study
3. Results and Discussion
3.1. Risk Assessment Studies
3.2. Optimization
3.3. Stock, Standard and Quality Control Sample
3.4. Method Validation
3.4.1. System Suitability
3.4.2. Linearity
3.4.3. Precision and Accuracy
3.4.4. Solution Stability
3.4.5. Robustness Study
4. Conclusions
Author Contributions
Funding
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Concn.(μg/mL) | Standard Stock Solution (mL) (BST) (μg/mL) | Internal Standard (mL) (ENC) (100 μg/mL) | Mobile Phase (mL) (A:B 60:40 v/v) | Total Volume (mL) |
---|---|---|---|---|
8 μg/mL (80%) | 0.16 | 0.4 | 1.44 | 2.0 |
10 μg/mL (100%) | 0.20 | 0.4 | 1.40 | 2.0 |
12 μg/mL (120%) | 0.24 | 0.4 | 1.36 | 2.0 |
Bosutinib Chromatographic Technique Features | |||||||
---|---|---|---|---|---|---|---|
CAAs | Eluent System Components | Wavelength of the Sensor | Column Temperature | Sample Volume | Flow Speed | Flow Pattern | Column Sizes |
Retention time | +1 | 0 | 0 | 0 | +1 | 0 | 0 |
Peak Area | +1 | 0 | −1 | 0 | +1 | −1 | 0 |
Tailing Factor | +1 | −1 | −1 | 0 | 0 | 0 | 0 |
S. No. | Independent Variable | Dependent Variable | |||
---|---|---|---|---|---|
Standard Run | Acetonitrile (%) | Flow Speed (mL/min) | Wavelength (nm) | Retention Time (min) | Tailing Factor |
1. | 35 | 0.8 | 260 | 1.87 | 0.88 |
2. | 45 | 0.8 | 255 | 1.89 | 0.87 |
3. | 35 | 1.2 | 260 | 1.83 | 0.93 |
4. | 45 | 1.2 | 260 | 1.98 | 0.88 |
5. | 35 | 1 | 250 | 1.92 | 0.94 |
6. | 45 | 1 | 250 | 1.93 | 0.88 |
7. | 35 | 1 | 270 | 1.84 | 0.9 |
8. | 45 | 1 | 270 | 1.97 | 0.91 |
9. | 40 | 0.8 | 250 | 1.98 | 0.86 |
10. | 40 | 1.2 | 250 | 1.95 | 0.92 |
11. | 40 | 0.8 | 270 | 1.89 | 0.87 |
12. | 40 | 1.2 | 270 | 1.98 | 0.88 |
13 *. | 40 | 1 | 260 | 1.92 | 0.89 |
14 *. | 40 | 1 | 260 | 1.92 | 0.89 |
15 *. | 40 | 1 | 260 | 1.92 | 0.89 |
16 *. | 40 | 1 | 260 | 1.92 | 0.89 |
17 *. | 40 | 1 | 260 | 1.92 | 0.89 |
Retention Time (min) | Tailing Factor | Plate Count | ||||
---|---|---|---|---|---|---|
BST | ENC | BST | ENC | BST | ENC | |
1 | 1.94 | 4.06 | 0.9 | 1.21 | 2032 | 4288 |
2 | 1.95 | 3.99 | 0.88 | 1.2 | 2018 | 4232 |
3 | 1.91 | 3.97 | 0.9 | 1.21 | 2013 | 4276 |
4 | 1.89 | 4.05 | 0.91 | 1.18 | 2012 | 4232 |
5 | 1.93 | 3.99 | 0.87 | 1.18 | 2022 | 4284 |
6 | 1.93 | 4.06 | 0.91 | 1.17 | 2003 | 4224 |
Average | 1.925 | 4.02 | 0.895 | 1.19167 | 2016.667 | 4256 |
SD | 0.0197906 | 0.03742 | 0.015 | 0.01572 | 9.012337 | 27.03085 |
%RSD | 0.98 | 0.92 | 1.68 | 1.26 | 4.46 | 0.63 |
S. No. | Parameters | Numerical Value |
---|---|---|
1 | Linearity range (µg mL−1) | 2–20 |
2 | Intercept | 0.109 |
3 | Slope | 0.561 |
4 | Correlation coefficient (r2) | 0.999 |
5 | SD | 0.098 |
6 | %RSD | 1.659 |
7 | LOD (µg mL−1) | 0.496 |
8 | LOQ (µg mL−1) | 1.503 |
Precision | ||||||
---|---|---|---|---|---|---|
Inter-Day | Intraday | |||||
Theoretical concentration (µg mL−1) | Concentration found | %RSD | Theoretical concentration (µg mL−1) | Concentration found | %RSD | |
LQC | 2 | 1.97 ± 0.037 | 1.892 | 2 | 2.08 ± 0.04 | 1.923 |
MQC | 12 | 11.91 ± 0.222 | 1.874 | 12 | 11.96 ± 0.21 | 1.762 |
HQC | 20 | 19.89 ± 0.342 | 1.723 | 20 | 19.91 ± 0.362 | 1.823 |
Accuracy (% Recovery) (Rat Plasma Samples) | ||||||
Excess drug added to analyte % | Theoretical Content (µg mL−1) | Concentration found (Mean ± SD) | % Recovery (Mean ± SD) | %RSD | ||
0 | 8 | 7.86 ± 0.213 | 98.25 ± 1.847 | 1.881 | ||
50 | 12 | 11.84 ± 0.517 | 98.66 ± 1.954 | 1.982 | ||
100 | 16 | 16.2 ± 0.673 | 101.25 ± 1.783 | 1.763 | ||
150 | 20 | 20.08 ± 0.382 | 100.4 ± 1.482 | 1.476 |
At 25 °C for 14 Days | At 2–8 °C for 30 Days | ||||||
---|---|---|---|---|---|---|---|
A | B | C | %RSD | A | B | C | %RSD |
12 | 11.85 ± 0.223 | 98.75 ± 1.852 | 1.875 | 12 | 11.81 ± 0.186 | 98.41 ± 1.624 | 1.651 |
Retention Time (min) | Tailing Factor | Plate Count | ||||
---|---|---|---|---|---|---|
BST | ENC | BST | ENC | BST | ENC | |
Ammonium acetate buffer pH 3.1 (Mobile phase A) | 1.93 | 4.08 | 0.85 | 1.21 | 2089 | 4421 |
Ammonium acetate buffer pH 2.9 (Mobile phase A) | 1.91 | 4.12 | 0.91 | 1.16 | 2098 | 4212 |
Flow rate at 0.9 mL min−1 | 1.90 | 3.95 | 0.92 | 1.22 | 1988 | 4098 |
Flow rate at 1.1 mL min−1 | 1.95 | 4.13 | 0.93 | 1.18 | 1997 | 4235 |
Detector wavelength at 258 nm | 1.93 | 3.98 | 0.86 | 1.23 | 2095 | 4312 |
Detector wavelength at 262 nm | 1.94 | 4.05 | 0.88 | 1.17 | 2084 | 4308 |
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Najmi, A.; Rehman, Z.u.; Alhazmi, H.A.; Albratty, M.M.; Majrashi, N.H.; Hakami, K.M.; Najmi, N.A.; Mobarki, A.A. Optimization of Chromatographic Conditions with QbD for Method Development and Validation of Bosutinib by HPLC: Applications in Dosage Forms and Rat Plasma Analysis. Separations 2023, 10, 346. https://doi.org/10.3390/separations10060346
Najmi A, Rehman Zu, Alhazmi HA, Albratty MM, Majrashi NH, Hakami KM, Najmi NA, Mobarki AA. Optimization of Chromatographic Conditions with QbD for Method Development and Validation of Bosutinib by HPLC: Applications in Dosage Forms and Rat Plasma Analysis. Separations. 2023; 10(6):346. https://doi.org/10.3390/separations10060346
Chicago/Turabian StyleNajmi, Asim, Zia ur Rehman, Hassan Ahmed Alhazmi, Mohammed Mofarreh Albratty, Nasser Hassan Majrashi, Khalid Mohammed Hakami, Naif Ali Najmi, and Ammar Abdullah Mobarki. 2023. "Optimization of Chromatographic Conditions with QbD for Method Development and Validation of Bosutinib by HPLC: Applications in Dosage Forms and Rat Plasma Analysis" Separations 10, no. 6: 346. https://doi.org/10.3390/separations10060346