Simultaneous Determination of Acrylamide, Caffeic Acid, and Caffeine in Commercial Coffee Capsules Using a Rapid and Validated HPLC-DAD Approach
Copyright © 2025 Wassila Belkhiri-Beder, Lamia Taouzinet, Zahra Toutou, Khodir Madani, Sofiane Fatmi
This work is licensed under a Creative Commons Attribution 4.0 International License.
- Attribution — You must give appropriate credit, provide a link to the license, and indicate if changes were made.
- No additional restrictions — You may not apply legal terms or technological measures that legally restrict others from doing anything the license permits.
Background: Coffee capsules are increasingly consumed worldwide and represent a complex source of bioactive compounds, notably caffeine (stimulant), caffeic acid (antioxidant), and acrylamide (toxicant).
Aims: The objectives of this investigation were twofold: (i) assess total phenolic content (TPC), antioxidant capacity, pH, and browning index, across seven commercial capsule products (comprising six Algerian brands widely consumed locally and one European comparator with undisclosed blend/roast); and (ii) to develop and validate an HPLC – Diode Array Detection (DAD) procedure for the simultaneous determination of caffeine, caffeic acid, and acrylamide , serving as joint indicators of product quality and safety.
Methods: The TPC was determined employing the Folin–Ciocalteu method, while antioxidant activity was assessed by the DPPH radical scavenging assay. The simultaneous quantification of caffeine, caffeic acid, and acrylamide were performed by a validated HPLC – DAD procedure in accordance with International Council for Harmonization (ICH) guidelines.
Results: The resulting coffee brews exhibited pH values ranging from 5.64 to 6.25 and browning indices between 0.280 and 0.482, reflecting roasting differences. Despite a modest TPC (0.9 to 2 mg GAE/g), the antioxidant activity was high, (up to 95.3% inhibition DPPH). Caffeine was consistently detected (0.05 – 0.33 mg/25 mL), confirming its stimulant role. Caffeic acid was present in lower concentrations (0.001 – 0.14 mg/25 mL), contributed to the antioxidant potential. In contrast, acrylamide was detected in all analyzed samples ranging from 4.75 to 28.15 µg/25 mL). On a dry coffee basis, these concentrations correspond to 458 – 4023 µg/kg. A majority of the capsules yielded levels that exceed the European Commission’s benchmark of 400 µg/kg for roasted coffee, thereby underscoring consumer-relevant exposure level and raising toxicological concern.
Conclusions: Coffee capsule brews demonstrated notable antioxidant capacity despite modest TPC, with caffeine ubiquitous and caffeic acid detectable. The presence of acrylamide was confirmed in all samples at levels that warrant monitoring. The validated HPLC–DAD workflow enables the simultaneous determination of these markers and offers a robust basis for integrated quality control and risk assessment in encapsulated coffee products.
Keywords
How to Cite
Bartel, C., Mesias, M., & Morales, F. J. (2015). Investigation on the extractability of melanoidins in portioned espresso coffee. Food Research International (Ottawa, Ont.), 67, 356–365. https://doi.org/10.1016/j.foodres.2014.11.053
Beder-Belkhiri, W., Zeghichi-Hamri, S., Kadri, N., Boulekbache-Makhlouf, L., Cardoso, S., Oukhmanou-Bensidhoum, S., & Madani, K. (2018). Hydroxycinnamic acids profiling, in vitro evaluation of total phenolic compounds, caffeine and antioxidant properties of coffee imported, roasted and consumed in Algeria. Mediterranean Journal of Nutrition and Metabolism, 11(1), 51–63. https://doi.org/10.3233/mnm-17181
Bekedam, E. K., Loots, M. J., Schols, H. A., Van Boekel, M. A. J. S., & Smit, G. (2008). Roasting effects on formation mechanisms of coffee brew melanoidins. Journal of Agricultural and Food Chemistry, 56(16), 7138–7145. https://doi.org/10.1021/jf800999a
Bekedam, E. K., Schols, H. A., van Boekel, M. A. J. S., & Smit, G. (2006). High molecular weight melanoidins from coffee brew. Journal of Agricultural and Food Chemistry, 54(20), 7658–7666. https://doi.org/10.1021/jf0615449
Cämmerer, B., & Kroh, L. W. (2006). Antioxidant activity of coffee brews. European Food Research and Technology, 223(4), 469–474. https://doi.org/10.1007/s00217-005-0226-4
Caporaso, N., Genovese, A., Canela, M. D., Civitella, A., & Sacchi, R. (2014). Neapolitan coffee brew chemical analysis in comparison to espresso, moka and American brews. Food Research International (Ottawa, Ont.), 61, 152–160. https://doi.org/10.1016/j.foodres.2014.01.020
Capuano, E., & Fogliano, V. (2011). Acrylamide and 5-hydroxymethylfurfurAL (HMF): A review on metabolism, toxicity, occurrence in food and mitigation strategies. Lebensmittel-Wissenschaft Und Technologie Food Science and Technology, 44(4), 793–810. https://doi.org/10.1016/j.lwt.2010.11.002
Clarke, R., & Vitzthum, O. G. (2001). Coffee: Recent developments (R. J. Clarke & O. G. Vitzthum, Eds.). Blackwell Science.
Clifford, M. N., Jaganath, I. B., Ludwig, I. A., & Crozier, A. (2017). Chlorogenic acids and the acyl-quinic acids: discovery, biosynthesis, bioavailability and bioactivity. Natural Product Reports, 34(12), 1391–1421. https://doi.org/10.1039/c7np00030h
Crozier, T. W. M., Stalmach, A., Lean, M. E. J., & Crozier, A. (2012). Espresso coffees, caffeine and chlorogenic acid intake: potential health implications. Food & Function, 3(1), 30–33. https://doi.org/10.1039/c1fo10240k
Similar Articles
- Efficacy of Moringa Soy Milk as a Food-Based Intervention on Hemoglobin Levels in Anemic Pregnant Women: A Quasi-Experimental Study in Gorontalo, Indonesia
- Bioactive molecules of grape
- Effect of traditional processing methods on protein digestibility and chemical constituents in seeds of Bauhinia petersiana
- Influence of Grain Size on the Agglomeration and Quality of Fine Couscous Derived from Decorticated White Sorghum Bicolor L.
- Physical properties and chemical composition of three Ethiopian rice (Oryza sativa Linn.) varieties compared to tef [Eragrostis tef (Zucc.) Trotter] grain
- Mediterranean diet and food consumption in an urban adult population of Northwest Algeria
- Quality of life, perceived stress and nutrition of patients with irritable bowel syndrome: A descriptive study
- Nutritional Status and Beverage Intake Patterns among Civil Servants in Southwestern Nigeria
- The Inhibitory Effect of Selenium Supplementation on Tumor Progression in a DMBA-Induced Breast Cancer Model in Wistar Rats
- Determination of isoflavones from soy-milk, masoor and mung dal soups in Bangladeshi postmenopausal women
You may also start an advanced similarity search for this article.
Most read articles by the same author(s)
- Impact of carob (Ceratonia Ciliqua L) pulp flour supplementation on probiotic viability, milk fermentation and antioxidant capacity during yogurt storage
- Ziziphus lotus (L.) Lam. plant treatment by ultrasounds and microwaves to improve antioxidants yield and quality: An overview
- Anticarcinogenic and antioxidant activities of leaves and flowers hydroalcoholic extracts of Nerium oleander L.: PCA analysis and phytochemical content by FTIR spectroscopy
- Development and characterization of sauces formulations based on tomato and garlic powders
- Impact of incorporating sesame oil (Sesamum indicum L.) in an Algerian frying oil and margarine formulation
- Microwave-assisted extraction optimization and conventional extraction of phenolic compounds from coriander leaves: UHPLC characterization and antioxidant activity
- Study of the relationship between nutrition, physical activity and overweight/obesity in children in a school context: Study of the relationship between nutrition, physical activity
- Ultrasound as pre-treatment for microwave drying of Myrtus communis fruits: Influence on phenolic compounds and antioxidant activity
- Physicochemical characterization and antioxidant capacity of the extracted oil from date pits and its effect on storage stability of margarine
- Advantages and Drawbacks of Plant-Based Beverages as Alternatives to Animal Milk: A Multidimensional Review
NAJFNR is licensed under 