Validation of a Novel RP-HPLC Technique for Simultaneous Estimation of Lignocaine Hydrochloride and Tibezonium Iodide: Greenness Estimation Using AGREE Penalties
Abstract
:1. Introduction
2. Results and Discussion
2.1. Method Development and Optimization
2.2. System Suitability
2.2.1. Retention Time
2.2.2. Resolution
2.2.3. Tailing Factor
2.2.4. Theoretical Plate Count
2.3. Method Validation
2.3.1. Linearity
2.3.2. Accuracy
2.3.3. Precision
2.3.4. Limit of Detection (LOD) and Limit of Quantification (LOQ)
2.3.5. Robustness
2.3.6. Specificity
2.4. In Vitro Dissolution Analysis
2.5. Salivary Drug Concentrations in Volunteers
2.6. Greenness of HPLC Method
3. Materials and Methods
3.1. Materials/Chemicals/Reagents
3.2. Instrumental Conditions
3.3. Mobile Phase Preparation
3.4. Standard Solution Preparation
3.5. System Suitability Parameters
3.5.1. Retention Time
3.5.2. Resolution
3.5.3. Tailing Factor
3.5.4. Theoretical Plate Count
3.6. Validation Parameters for the Proposed Method
3.6.1. Linearity
3.6.2. Accuracy
3.6.3. Precision
3.6.4. Limit of Detection (LOD) and Limit of Quantification (LOQ)
3.6.5. Robustness
3.6.6. Specificity
3.7. In Vitro Dissolution Studies
3.8. Salivary Drug Concentration
3.9. Greenness of HPLC Method
3.10. Statistical Analysis
4. Conclusions
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 | Tibezonium Iodide | Lignocaine Hydrochloride |
---|---|---|
System Suitability Parameters | ||
Retention time (min) | 4.20 ± 0.28 | 2.33 ± 0.18 |
Tailing factor | 1.86 | 1.32 |
Peak area | 70.32 ± 0.74 | 98.97 ± 0.84 |
Theoretical plates (USP) | 5598 | 4339 |
Resolution | 2.591 | --- |
Linearity Parameters | ||
Linear function | y = 26.321x + 0.7419 | y = 1.9737x − 0.5297 |
Regression coefficient (r2) | 0.9995 | 0.9992 |
Linearity range (µg/mL) | 0.14–10.08 | 0.28–20.18 |
LOD (µg/mL) | 0.011 | 0.115 |
LOQ (µg/mL) | 0.037 | 0.384 |
Percent Level | Tibezonium Iodide | Lignocaine Hydrochloride | ||||||
---|---|---|---|---|---|---|---|---|
Theoretical Content (µg/mL) | Amount Recovered (µg/mL) | Recovery (%) | RSD (%) | Theoretical Content (µg/mL) | Amount Recovered (µg/mL) | Recovery (%) | RSD (%) | |
80% | 8.96 | 8.91 | 99.34 | 1.46 | 4.48 | 1.83 | 100.12 | 0.75 |
100% | 11.2 | 11.15 | 100.01 | 1.72 | 5.6 | 2.56 | 99.05 | 0.65 |
120% | 13.44 | 14.44 | 100.50 | 1.69 | 6.72 | 3.42 | 99.74 | 0.90 |
Percent Level | Tibezonium Iodide | Lignocaine Hydrochloride | ||||||
---|---|---|---|---|---|---|---|---|
Percent Precision | Intraday RSD (%) | Percent Precision | Interday RSD (%) | Percent Precision | Intraday RSD (%) | Percent Precision | Interday RSD (%) | |
80% | 99.34 | 1.83 | 98.63 | 1.75 | 100.42 | 0.96 | 99.89 | 1.46 |
100% | 100.03 | 1.61 | 99.14 | 0.65 | 99.05 | 0.48 | 99.19 | 1.72 |
120% | 100.10 | 1.65 | 99.01 | 0.90 | 99.84 | 0.77 | 98.84 | 1.69 |
Parameters | Tibezonium Iodide Content % (RSD %) | Lignocaine HCl Content % (RSD %) |
---|---|---|
Optimal condition | ||
1.00 mL/min, 35 °C, pH 4.5 | 99.83 (1.52) | 98.46 (0.65) |
Flow rate variation | ||
0.85 mL/min | 97.79 (1.24) | 99.57 (0.91) |
1.15 mL/min | 98.11(1.86) | 98.36 (0.62) |
Temperature variation | ||
30 °C | 98.60 (0.22) | 99.93 (0.31) |
40 °C | 98.37 (0.29) | 99.50 (0.24) |
pH variation | ||
pH 4.0 | 99.19 (1.91) | 100.42 (1.78) |
pH 5.0 | 100.02 (1.81) | 99.26 (1.91) |
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Hanif, S.; Syed, M.A.; Rashid, A.J.; Alharby, T.N.; Algahtani, M.M.; Alanazi, M.; Alanazi, J.; Sarfraz, R.M. Validation of a Novel RP-HPLC Technique for Simultaneous Estimation of Lignocaine Hydrochloride and Tibezonium Iodide: Greenness Estimation Using AGREE Penalties. Molecules 2023, 28, 3418. https://doi.org/10.3390/molecules28083418
Hanif S, Syed MA, Rashid AJ, Alharby TN, Algahtani MM, Alanazi M, Alanazi J, Sarfraz RM. Validation of a Novel RP-HPLC Technique for Simultaneous Estimation of Lignocaine Hydrochloride and Tibezonium Iodide: Greenness Estimation Using AGREE Penalties. Molecules. 2023; 28(8):3418. https://doi.org/10.3390/molecules28083418
Chicago/Turabian StyleHanif, Sana, Muhammad Ali Syed, Ahmad Junaid Rashid, Tareq Nafea Alharby, Mohammad M. Algahtani, Muteb Alanazi, Jowaher Alanazi, and Rai Muhammad Sarfraz. 2023. "Validation of a Novel RP-HPLC Technique for Simultaneous Estimation of Lignocaine Hydrochloride and Tibezonium Iodide: Greenness Estimation Using AGREE Penalties" Molecules 28, no. 8: 3418. https://doi.org/10.3390/molecules28083418