Research Article
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Year 2023, , 485 - 490, 29.09.2023
https://doi.org/10.17776/csj.1319590

Abstract

References

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  • [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.

Determination of Caffeine in Human Plasma by Using Liquid Chromatography-Tandem Mass Spectrometry

Year 2023, , 485 - 490, 29.09.2023
https://doi.org/10.17776/csj.1319590

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.

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.
There are 11 citations in total.

Details

Primary Language English
Subjects Pharmaceutical Analytical Chemistry
Journal Section Natural Sciences
Authors

Fırat Yerlikaya 0000-0003-4648-3258

Onursal Sağlam 0000-0002-1421-6633

Publication Date September 29, 2023
Submission Date June 24, 2023
Acceptance Date August 28, 2023
Published in Issue Year 2023

Cite

APA Yerlikaya, F., & Sağlam, O. (2023). Determination of Caffeine in Human Plasma by Using Liquid Chromatography-Tandem Mass Spectrometry. Cumhuriyet Science Journal, 44(3), 485-490. https://doi.org/10.17776/csj.1319590