UHPLC-MS/MS quantification of atractyligenin glycosides in Arabica coffee and coffee brew

The data comprise the raw data to the publication "UHPLC-MS/MS quantification of atractyligenin glycosides in Arabica coffee and coffee brew" submitted to the "Journal of Food Composition and Analysis".
Find the article here: https://doi.org/10.1016/j.jfca.2025.107432

Atractyligenin and its glycosides are coffee-specific diterpene glycosides with particular abundance in C. arabica, C. liberica, and C. stenophylla. We developed a UHPLC-MS/MS method and sample extraction protocol for their quantification in roasted coffee samples. During method development, we assessed the linear range, instrumental Limit of Detection and Limit of Quantification, and precision and accuracy in spiked analyte-free liquid and solid matrix. We evaluated precision and repeatability in authentic samples. Aqueous extraction approximated completion after 30 min of incubation at 95°C. We analyzed a sample set of Arabica coffee from Colombia and coffee brews using the method. The data showed that Arabica coffee from Colombia contained 2.2 – 4.1 µmol/g atractyligenin derivatives. 2-O-β-D-glucosylatractyligenin was the principal constituent (46.8 - 63.6%), followed by 3'-O-β-D-glucosyl-2'-O-isovaleryl-2-O-β-D-glucosylatractyligenin (18.9 - 35.7%). Atractyligenin accounted for 5.5 - 14.8% and 2'-O-isovaleryl-2-O-β-D-glucosylatractyligenin for 6.0 - 12.1%. The four compounds were nearly quantitatively extracted during coffee brewing. Extraction rates were 79.1 - 98.3%.
The data show that these coffee-specific diterpenoids are extracted and ingested with the coffee brew. After ingestion atractyligenin glycosides are subject to metabolic breakdown, leading to coffee-specific metabolites, e.g., atractyligenin-19-O-glucuronide, in the plasma and urine.
In conclusion these coffee-specific diterpenoids form coffee-specific metabolites that could be exploited as dietary biomarkers indicating recent coffee consumption. Such dietary biomarkers are of importance in nutritional intervention studies on, e.g., the health impact of regular coffee consumption.
- NMR spectra of the compounds 2´-O-isovaleryl-2-O-β-D-glucosylatractyligenin obtained by acidic hydrolysis of atractyloside
- NMR spectra of the compounds 2´-O-isovaleryl-2-O-β-D-glucosylcarboxyatractyligenin obtained by acidic hydrolysis of 4´-desulfocarboxyatractylic acid
- validation data of the developed UHPLC-MS/MS method (linear range, LoD. LoQ, precision and accuracy in analyte-free matrix, precision in authentic samples)
- quantitative data on the concentrations of atractyligenin and its glycosides in roasted Arabica coffee from Colombia and coffee brews (French Press, Turkish coffee, Espresso coffee, Cold Brew).
- experimental data on lipophilicity of atractyligenin and its glycosides in terms of water:n-octanol coefficient.