Method Validation for Determination of Caffeine in Sidomulyo Robusta Coffee Beans Using Gas Chromatography-Flame Ionization Detector

Article Preview

Abstract:

Caffeine, an alkaloid compound found in coffee, is widely known for its ability to stimulate the human central nervous system. The caffeine content in Sidomulyo robusta coffee was analyzed using a gas chromatography-flame ionization detector (GC-FID) with ultrasound-assisted extraction as a preparation method using methanol solvent for 21 minutes at 32°C. A TR-1MS column (15m x 0.25 mm ID x 0.25 μm film, non-polar column 100% dimethyl poly-siloxane) was used for the GC analysis. The injector temperature was set at 260°C and the detector at 280°C. The initial oven temperature was set at 100°C, held for 1 minute, then gradually increased by 5°C/minute up to 280°C and held for 2 minutes, with the optimal flow rate condition selected at 1.2 mL/min. This method met all verification criteria and exhibited linearity in the 100–600 mg/L range with a high correlation coefficient of 0.9929, demonstrating its reliability and accuracy in determining caffeine content in coffee samples

You might also be interested in these eBooks

Info:

Periodical:

Engineering Headway (Volume 24)

Pages:

47-56

Citation:

Online since:

July 2025

Export:

Price:

Permissions CCC:

Permissions PLS:

Сopyright:

© 2025 Trans Tech Publications Ltd. All Rights Reserved

Share:

Citation:

* - Corresponding Author

[1] Mendoza, M. F., Sulague, R. M., Posas-mendoza, T., & Lavie, C. J. (2023). Impact of Coffee Consumption on Cardiovascular Health, 152–158

DOI: 10.31486/toj.22.0073

Google Scholar

[2] Al-bratty, M., Alhazmi, H. A., Rehman, Z., Javed, S. A., Ahsan, W., Najmi, A., … Khalid, A. (2020). Determination of Caffeine Content in Commercial Energy Beverages Available in Saudi Arabian Market by Gas Chromatography-Mass Spectrometric Analysis, 2020(2008).

DOI: 10.1155/2020/3716343

Google Scholar

[3] Hameed, A., Hussain, S. A., Ansar, H., & Suleria, R. (2018). " Coffee Bean-Related " Agroecological Factors Affecting the Coffee.

DOI: 10.1007/978-3-319-76887-8_21-1

Google Scholar

[4] Farikha, I. A., Eka, L., Rahayuningtyas, A., & Ulum, B. (2025). Determination of Caffeine Content at the Difference in Arabica and Robusta Coffee Roast Levels Using HPLC, 04011.

DOI: 10.1051/bioconf/202515804011

Google Scholar

[5] Atlabachew, M., Habtemariam, Y. T., Abebe, A., & Wubieneh, T. A. (2021). Rapid and simultaneous determination of trigonelline , caffeine , and chlorogenic acid in green coffee bean extract, (June), 1–8

DOI: 10.1002/fsn3.2456

Google Scholar

[6] Pasias, I. N., Kiriakou, I., & Proestos, C. (2017). Development of a Rapid Method for the Determination of Caffeine in Coffee Grains by GC-FID — A Fully Validated Approach, 4–9

DOI: 10.3390/antiox6030067

Google Scholar

[7] Misra, B. B., Bassey, E., & Olivier, M. (2019). Comparison of a GC-Orbitrap-MS with Parallel GC-FID Capabilities for Metabolomics of Human Serum.

DOI: 10.1101/740795

Google Scholar

[8] Prabhune, S., Limited, C., Dighe, V. D., & Limited, H. F. (2015). Enantiomeric Separation Of Rivaroxaban by a Chiral Liquid Chromatographic Method Original Article Innovare Enantiomeric Separation of Rivaroxaban By A Chiral Liquid Chromatographic, (February).

DOI: 10.31274/rtd-20200803-354

Google Scholar

[9] He, D., Huang, Y., Ayupdek, D., Gu, Y., Yaang, Y., Aisyah, H.A., 7 Ito, Y. (2011). Sepratation and Purification of Flavonoids from Black Currant Leaves by High Speed Counter current Chromatography and Preparative HPLC. NIH Public Access, 33(5), 615–628.

DOI: 10.1080/10826071003608447

Google Scholar

[10] Kunarto, B., Sutardi, Surpiyanto,and Anwar, C. (2019). Optimasi Ekstraksi Berbantu Gelombang Ultrasonik pada Biji Melinjo Kerikil (Gnetum gnemon L., 'Kerikil') Menggunakan Response Surface Methodology, 8(3), 1–8.

DOI: 10.17728/jatp.5122

Google Scholar

[11] Uddin, M.S., Ferdosh, S., Akanda, J. H., Ghafoor, K., & Rukshana, A. H. (2018). Techniques for the extraction of phytosterols and their benefits in human health : a review.

Google Scholar

[12] Harmono, H.D. (2020). Validasi Metode Analisis Logam Merkuri ( Hg ) Terlarut pada Air Permukaan dengan Automatic Mercury Analyzer ISSN 2655 4887 ( Print ), ISSN 2655 1624 ( Online ) ISSN 2655 4887 ( Print ), ISSN 2655 1624 ( Online ), 2(3), 11–16.

DOI: 10.22146/ijl.v2i3.57047

Google Scholar

[13] Belouafa, S., Habti, F., Benhar, S., Belafkih, B., Tayane, S., & Hamdouch, S. (2017). Statistical tools and approaches to validate analytical methods : methodology and practical examples ★, 9

DOI: 10.1051/ijmqe/2016030

Google Scholar

[14] Zambakjian, C. (2020). A new gas chromatographic method development and validation for the simultaneous determination of ibuprofen and caffeine in bulk and pharmaceutical dosage form, 0.

DOI: 10.1186/s43094-020-00123-0

Google Scholar

[15] Marthia, N., (2021). PEMISAHAN KAFEIN DENGAN METODE MICROWAVE ASSISTED EXTRACTION ( MAE ) TERHADAP 4 JENIS BIJI KOPI ROBUSTA, 8(2), 51–55.

DOI: 10.23969/pftj.v8i2.4172

Google Scholar

[16] Bakalyar, S.R, & Hendry, R, A. and gradient analysis, while sampIe size and column temper- ature were held constant. The resulting peak behavior was observed and compared with tkeory. General guidelines were developed.

Google Scholar

[17] Ravisankar, P., Navya, C. N., Pravallika, D., & Sri, D. N. (2015). A Review on Step-by-Step Analytical Method Validation, 5(10), 7–19.

Google Scholar

[18] Janson, J. (2011). Protein purification: principles, High Resolution Methods, and Aplication, Willey, USA

Google Scholar

[19] Regmi, B. P., & Agah, M. (2018). Micro Gas Chromatography: An Overview of Critical Components and Their Integration

DOI: 10.1021/acs.analchem.8b01461

Google Scholar

[20] Wichitnithad, W., Sudtanon, O., Srisunak, P., Cheewatanakornkool, K., Nantaphol, S., & Rojsitthisak, P. (2021). Development of a Sensitive Headspace Gas Chromatography − Mass Spectrometry Method for the Simultaneous Determination of Nitrosamines in Losartan Active Pharmaceutical Ingredients

DOI: 10.1021/acsomega.1c00982

Google Scholar

[21] Susanty, & Bachmid, F. Perbandingan Metode Ekstraksi Maserasi dan Refluks terhadap Kadar Fenolik dari Ekstrak Tongkol Jagung (Zea mays L.) (Susanty, Fairus Bachmid), 87–93.

DOI: 10.24853/konversi.5.2.87-92

Google Scholar

[22] Caracostea, L.-M. (2021). Determination of Caffeine Content in Arabica and Robusta Green Coffee of Indian Origin, 8705(June), 69–79.

DOI: 10.26417/425qba31z

Google Scholar

[23] Jeszka, M., Aleksandra, S., & Krystyna, S. (2016). Chlorogenic acids , caffeine content and antioxidant properties of green coffee extracts : influence of green coffee bean preparation

DOI: 10.1007/s00217-016-2643-y

Google Scholar

[24] Ihsan, B.R.P., Shalas, A.F., Elisabeth, Y., Claudia, L.M., 7 Putri A.R. (2023). Determination of caffeine in Robusta coffee beans with different roasting, 7(December), 29–34.

DOI: 10.26656/fr.2017.7(6).1006

Google Scholar