A Green High-Performance Thin-Layer Chromatography Method for the Determination of Caffeine in Commercial Energy Drinks and Formulations
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Chromatography and Analytical Conditions
2.3. Preparation of Caffeine Standard Solutions for Calibration and Quality Control (QC) Samples
2.4. Sample Processing of Caffeine from Marketed ED
2.5. Processing of Samples for the Determination of Caffeine in Marketed Herbal Products
2.6. Validation Parameters
2.7. Determination of Caffeine in Marketed ED and Herbal Products
2.8. Greenness Assessment
3. Results and Discussion
3.1. Method Development
3.2. Validation Parameters
3.3. Determination of Caffeine in Marketed ED and Herbal Products
3.4. Greenness Assessment
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
References
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Parameters | Values |
---|---|
Linearity range (ng band−1) | 50–800 |
Regression equation | y = 28.429x + 813.89 |
R2 | 0.9973 |
R | 0.9986 |
SE of slope | 0.35 |
SE of intercept | 2.42 |
95% CI of slope | 26.90–29.95 |
95% CI of intercept | 803.45–824.32 |
LOD ± SD (ng band−1) | 16.87 ± 0.45 |
LOQ ± SD (ng band−1) | 50.61 ± 1.35 |
Parameters | Green HPTLC Method |
---|---|
Rf | 0.42 ± 0.01 |
As | 1.06 ± 0.02 |
N m−1 | 5241 ± 4.58 |
Conc. (ng Band−1) | Conc. Found (ng Band−1) ± SD | Recovery (%) | CV (%) |
---|---|---|---|
100 | 98.52 ± 1.36 | 98.5 | 1.38 |
500 | 508.23 ± 3.54 | 101.6 | 0.69 |
800 | 788.36 ± 6.94 | 98.5 | 0.88 |
Conc. (ng Band−1) | Intraday Precision | Interday Precision | ||||
---|---|---|---|---|---|---|
Conc. Found (ng Band−1) ± SD | Standard Error | CV (%) | Conc. Found (ng Band−1) ± SD | Standard Error | CV (%) | |
100 | 101.45 ± 0.84 | 0.34 | 0.82 | 99.21 ± 0.92 | 0.37 | 0.92 |
500 | 494.31 ± 3.11 | 1.26 | 0.62 | 491.23 ± 3.53 | 1.44 | 0.71 |
800 | 792.34 ± 4.74 | 1.93 | 0.59 | 806.32 ± 5.15 | 2.10 | 0.63 |
Conc. (ng Band−1) | Mobile Phase Composition (EtOH-Water) | Results | ||||
---|---|---|---|---|---|---|
Original | Used | Conc. (ng Band−1) ± SD | CV (%) | Rf | ||
57:43 | +2.0 | 492.54 ± 3.22 | 0.65 | 0.41 | ||
500 | 55:45 | 55:45 | 0.0 | 504.51 ± 3.66 | 0.72 | 0.42 |
53:47 | −2.0 | 511.21 ± 3.97 | 0.77 | 0.43 |
Samples | Label Content of Caffeine (mg 100 mL−1) | Caffeine Found (mg 100 mL−1) | Percent of Label Amount |
---|---|---|---|
ED1 | 30 | 30.52 ± 1.01 | 98.2 |
ED2 | 30 | 29.19 ± 1.00 | 102.7 |
ED3 | 32 | 31.21 ± 1.03 | 102.5 |
ED4 | 32 | 32.89 ± 1.04 | 97.2 |
ED5 | 30 | 28.08 ± 1.01 | 106.8 |
ED6 | 20 | 21.02 ± 0.80 | 95.1 |
ED7 | 32 | 31.88 ± 2.02 | 100.3 |
ED8 | 30 | 29.98 ± 1.01 | 100.0 |
ED9 | 35 | 37.52 ± 2.01 | 93.2 |
ED10 | 35 | 35.93 ± 2.04 | 97.3 |
F1 | 10 | 10.63 ± 0.50 | 94.0 |
F2 | 20 | 20.30 ± 0.60 | 98.4 |
F3 | 15 | 15.92 ± 0.65 | 94.2 |
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Foudah, A.I.; Shakeel, F.; Salkini, M.A.; Alshehri, S.; Ghoneim, M.M.; Alam, P. A Green High-Performance Thin-Layer Chromatography Method for the Determination of Caffeine in Commercial Energy Drinks and Formulations. Materials 2022, 15, 2965. https://doi.org/10.3390/ma15092965
Foudah AI, Shakeel F, Salkini MA, Alshehri S, Ghoneim MM, Alam P. A Green High-Performance Thin-Layer Chromatography Method for the Determination of Caffeine in Commercial Energy Drinks and Formulations. Materials. 2022; 15(9):2965. https://doi.org/10.3390/ma15092965
Chicago/Turabian StyleFoudah, Ahmed I., Faiyaz Shakeel, Mohammad A. Salkini, Sultan Alshehri, Mohammed M. Ghoneim, and Prawez Alam. 2022. "A Green High-Performance Thin-Layer Chromatography Method for the Determination of Caffeine in Commercial Energy Drinks and Formulations" Materials 15, no. 9: 2965. https://doi.org/10.3390/ma15092965