Non-Destructive Analysis of Chlorpheniramine Maleate Tablets and Granules by Chemometrics-Assisted Attenuated Total Reflectance Infrared Spectroscopy
Abstract
:1. Introduction
2. Results
2.1. ATR-IR Measurement
2.2. HPLC Method and Method Validation
2.3. PLSR Modelling
2.4. Quantitative Determination of CPM Tablets and Granules by PLSR and HPLC Methods
3. Discussion
4. Conclusions
5. Experimental
5.1. Chemicals and Reagents
5.2. Preparation of Chlorpheniramine Maleate Tablets
5.3. ATR-IR Measurement
5.4. HPLC Analysis
5.5. PLSR Modeling
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Method Validation Characteristics | Results |
---|---|
Range | 10–30 µg/mL |
Linearity | |
Equation | y = 14,603x − 2363 |
R2 (n = 3) | 0.9999 |
Accuracy (% Recovery) | 100.0–102.9% |
Precision | |
Repeatability (n = 9) | 1.26 |
Intermediate precision (n = 18) | 1.13 |
Specificity | |
Peak purity index (standard) | 1.0000 |
Peak purity index (standard spiked placebo) | 0.9999 |
Model Number | Spectral Range (cm−1) | Spectral Data * | Latent Factors | R2 (Model) | R2 (Pearson) | RMSEC | RMSEP | Bias | Derivative Polynomial Order |
---|---|---|---|---|---|---|---|---|---|
1 | 400–4000 | original | 5 | 0.9142 | 0.9328 | 2.5419 | 2.4797 | 0.1986 | - |
2 | 400–4000 | D2 | 9 | 0.9545 | 0.9309 | 1.8506 | 2.4850 | −0.0359 | - |
3 | 400–4000 | area-normalized | 4 | 0.9083 | 0.9287 | 2.6284 | 2.5648 | 0.1862 | - |
4 | 400–4000 | area-normalized + SNV | 3 | 0.9355 | 0.9438 | 2.2040 | 2.2418 | 0.2695 | - |
5 | 2700–4000 | area-normalized + SNV | 5 | 0.9605 | 0.9591 | 1.7251 | 2.0673 | −0.1105 | - |
6 | 400–4000 | D1 | 5 | 0.9264 | 0.9312 | 2.3546 | 2.478 | −0.0123 | 2 order 11 pt. |
7 | 400–4000 | D1 + SNV | 9 | 0.9394 | 0.941 | 2.1359 | 2.3093 | −0.2371 | 2 order 11 pt. |
8 | 500–1700 | D2 | 7 | 0.9716 | 0.9417 | 1.4625 | 2.2801 | −0.3258 | 2 order 11 pt. |
9 | 2500–4000 | D2 | 5 | 0.9823 | 0.9579 | 1.1555 | 2.0986 | −0.1973 | 2 order 11 pt. |
10 | 500–1700, 2500–4000 | D2 | 7 | 0.9840 | 0.9562 | 1.0986 | 2.0155 | −0.415 | 2 order 11 pt. |
11 | 500–1700 | area-normalized + SNV | 8 | 0.9741 | 0.9639 | 1.3977 | 1.7611 | 0.0495 | - |
12 | 2500–4000 | area-normalized + SNV | 8 | 0.9481 | 0.9508 | 1.9759 | 2.1874 | −0.1130 | - |
13 | 500–1700, 2500–4000 | area-normalized + SNV | 8 | 0.9716 | 0.9632 | 1.4616 | 1.7786 | 0.0176 | - |
Model Number | Spectral Range (cm−1) | Spectral Data * | Latent Factors | R2 (Model) | R2 (Pearson) | RMSEC | RMSEP | Bias | Derivative Polynomial Order |
---|---|---|---|---|---|---|---|---|---|
1 | 400–3700 | Original | 2 | 0.9498 | 0.9762 | 15.0802 | 10.6003 | −2.0409 | - |
2 | 400–1700, 2800–3700 | Original 2 | 2 | 0.9395 | 0.9782 | 16.5568 | 10.1016 | −1.8677 | - |
3 | 400–3700 | SNV | 1 | 0.9366 | 0.9835 | 16.9389 | 8.6349 | −0.3478 | - |
4 | 400–1700, 2800–3700 | SNV | 1 | 0.9355 | 0.9838 | 17.0872 | 8.5433 | −0.3631 | - |
5 | 400–3700 | Area normalization | 2 | 0.9295 | 0.9730 | 17.8691 | 11.2178 | −2.0792 | - |
6 | 400–3700 | SNV + D1 | 2 | 0.9577 | 0.9858 | 13.8447 | 8.0012 | −0.4014 | 2 order 11 pt. |
7 | 400–3700 | SNV + D1 | 2 | 0.9572 | 0.9851 | 13.9199 | 8.4352 | −0.6258 | 2 order 21 pt. |
8 | 400–3700 | SNV + D1 | 1 | 0.9362 | 0.9833 | 16.9942 | 8.6657 | −0.3323 | 3 order 11 pt. |
9 | 400–3700 | SNV + D1 | 1 | 0.9364 | 0.9834 | 16.9678 | 8.6601 | −0.3574 | 3 order 21 pt. |
10 | 400–3700 | SNV + D1 | 1 | 0.9368 | 0.9835 | 16.9125 | 8.6220 | −0.3550 | 4 order 11 pt. |
11 | 400–3700 | SNV + D1 | 1 | 0.9368 | 0.9835 | 16.9196 | 8.6263 | −0.3573 | 4 order 21 pt. |
Active Content (%) | Tablets Model | Granules Model | ||
---|---|---|---|---|
Calibration | Validation | Calibration | Validation | |
4 | 24 | 6 | 7 | 3 |
8 | 24 | 6 | 7 | 3 |
12 | 24 | 6 | 7 | 3 |
15 | 24 | 6 | 7 | 3 |
20 | 24 | 6 | 7 | 3 |
25 | 24 | 6 | 7 | 3 |
30 | 24 | 6 | 7 | 3 |
Total | 168 | 42 | 49 | 21 |
Composition (mg/Tablet) | Formulation | ||||||
---|---|---|---|---|---|---|---|
1 | 2 | 3 | 4 | 5 | 6 | 7 | |
CPM | 4.0 | 8.0 | 10.0 | 15.0 | 20.0 | 25.0 | 30.0 |
Lactose monohydrate | 80.0 | 76.0 | 74.0 | 69.0 | 64.0 | 59.0 | 54.0 |
Tapioca starch | 40.0 | 40.0 | 40.0 | 40.0 | 40.0 | 40.0 | 40.0 |
Croscarmellose sodium | 3.7 | 3.7 | 3.7 | 3.7 | 3.7 | 3.7 | 3.7 |
Corn starch | 3.6 | 3.6 | 3.6 | 3.6 | 3.6 | 3.6 | 3.6 |
Magnesium stearate | 0.7 | 0.7 | 0.7 | 0.7 | 0.7 | 0.7 | 0.7 |
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Phechkrajang, C.; Khongkaew, P.; Limwikrant, W.; Jaturanpinyo, M. Non-Destructive Analysis of Chlorpheniramine Maleate Tablets and Granules by Chemometrics-Assisted Attenuated Total Reflectance Infrared Spectroscopy. Molecules 2022, 27, 3760. https://doi.org/10.3390/molecules27123760
Phechkrajang C, Khongkaew P, Limwikrant W, Jaturanpinyo M. Non-Destructive Analysis of Chlorpheniramine Maleate Tablets and Granules by Chemometrics-Assisted Attenuated Total Reflectance Infrared Spectroscopy. Molecules. 2022; 27(12):3760. https://doi.org/10.3390/molecules27123760
Chicago/Turabian StylePhechkrajang, Chutima, Putthiporn Khongkaew, Waree Limwikrant, and Montree Jaturanpinyo. 2022. "Non-Destructive Analysis of Chlorpheniramine Maleate Tablets and Granules by Chemometrics-Assisted Attenuated Total Reflectance Infrared Spectroscopy" Molecules 27, no. 12: 3760. https://doi.org/10.3390/molecules27123760