Abstract
References
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Abstract
A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to determine caffeine (CAF) in human plasma. The plasma samples were extracted by protein precipitation using CAF-D3 as an internal standard (IS). The chromatographic separation was performed on GL Sciences InertSustain C18 Column (4.6 x 50 mm, 5 µm) maintained at 40 °C with a mobile phase consisting of formic acid, water, and methanol at a 1 mL/min of flow rate using two separate lines. CAF was detected and identified by mass spectrometry with electrospray ionization (ESI) in positive ions and multiple-reaction monitoring (MRM) mode. The MRM transitions of m/z 195.10 > 138.00 for CAF and 198.10 > 141.10 for IS were used for quantification. The standard curve was linear in the range of 10 - 10000 ng/mL for CAF. The within-batch precision and accuracy were evaluated by analyzing QC samples at five different concentration levels with six replicates in a batch. The between-batch precision and accuracy were determined by analyzing three different batches. The within-batch accuracy and precision was -8.76% - 9.61% and 0.95% - 7.22%, respectively. The between-batch accuracy and precision was -7.47% -1.42% and 1.83% - 8.66%, respectively. The results of the intra- and inter-day precision and accuracy studies were within the limits. The validated method applied to a pharmacokinetic study and the test product containing 60 mg CAF administered to total of 12 subjects. The mean ± SD of maximum plasma concentration (Cmax) was found to be 147.94 ± 139.39 ng/mL and the mean ± SD of area under the plasma concentration-time curve from zero to last measurable concentration (AUC0-tlast) was found to be 1119.59 ± 1468.30 h.ng/mL for the fasting conditions. The median time to reach peak plasma concentration (Tmax) was found to be 12.00 (6.50 - 12.00). The developed and validated method can be used for bioavailability and bioequivalence studies in human plasma samples.
Keywords
References
- [1] Nehlig A., Daval JL., Debry G., Caffeine and the central nervous system: mechanisms of action, biochemical, metabolic and psychostimulant effects, Brain Research Reviews, 17 (2) (1992) 139-170.
- [2] Guest N.S., VanDusseldorp T.A., Nelson M.T., International society of sports nutrition position stand: caffeine and exercise performance, J Int Soc Sports Nutr., 18 (1) (2021).
- [3] PubChem Compound Summary for CID 2519, Caffeine, National Center for Biotechnology Information, (2023). Available at: https://pubchem.ncbi.nlm.nih.gov/compound/caffeine. Retrieved June 24, 2023.
- [4] De Maria C.A.B., Moreira R.F.A., Analytical methods for caffeine, Química Nova, 30 (1) (2007) 99-105.
- [5] Alvi S.N., Hammami M.M., Validated HPLC method for determination of caffeine level in human plasma using synthetic plasma: application to bioavailability studies, J Chromatogr Sci., 49 (4) (2011) 292-6.
- [6] Wang Y.H., Mondal G., Butawan M., Bloomer R.J., Yates C.R., Development of a liquid chromatography-tandem mass spectrometry (LC–MS/MS) method for characterizing caffeine, methylliberine, and theacrine pharmacokinetics in humans, Journal of Chromatography B, 1155 (2020).
- [7] Lu J.L., et al., Determination of purine alkaloids and catechins in different parts of Camellia assamica var. kucha by HPLC-DAD/ESI-MS/MS, J. Sci. Food Agric. 89 (2009) 2024–2029.
- [8] Li Y.F., et al., A comparative analysis of chemical compositions in Camellia sinensis var. puanensis Kurihara, a novel Chinese tea, by HPLC and UFLC-Q-TOF-MS/MS, Food Chemistry, 216 (2017) 282–288.
- [9] U.S. Department of Health and Human Services, Food and Drug Administration (FDA). Guidance for Industry. Bioanalytical Method Validation, (2018). Available at: https://www.fda.gov/media/70858/download. Retrieved June 24, (2023).
- [10] European Medicines Agency (EMA), Committee for Medicinal Product for Human Use (CHMP), Guideline on Bioanalytical Method Validation, (2022). Available at: https://www.ema.europa.eu/en/ich-m10-bioanalytical-method-validation-scientific-guideline. Retrieved August 23, (2023).
- [11] Grzegorzewski J., Bartsch F., Köller A. and König M., Pharmacokinetics of caffeine: A systematic analysis of reported data for application in metabolic phenotyping and liver function testing, Frontiers in Pharmacology, 12 (2022) 752826.
Details
| Primary Language | English |
|---|---|
| Subjects | Pharmaceutical Analytical Chemistry |
| Journal Section | Natural Sciences |
| Authors | |
| Publication Date | September 29, 2023 |
| Submission Date | June 24, 2023 |
| Acceptance Date | August 28, 2023 |
| Published in Issue | Year 2023Volume: 44 Issue: 3 |
