USP Standards for Dietary Ingredients Derived from Mate and Guayusa Leaves: A Quality by Design Approach to Method Development and Validation for the Simultaneous Determination of Methylxanthines and Hydroxycinnamoylquinic Acids
Year: 2026
Type: article
Abstract: ), both members of the Aquifoliaceae family and traditionally consumed as herbal teas in South America, are rich in methylxanthines and hydroxycinnamoylquinic acids that may provide stimulant and antioxidant properties for use in beverages and dietary supplements. This work demonstrates an analytical quality-by-design (AQbD) approach to developing a UHPLC method and sample preparation procedure for the simultaneous quantification of these compounds in mate and guayusa leaves and their extracts. Using AQbD principles, critical method attributes and parameters were defined and optimized through design of experiments to understand variable interactions, establish robustness within the method operable design region, and experimentally confirm the selected conditions. The resulting UHPLC-DAD method separates three methylxanthines and nine hydroxycinnamoylquinic acids within 12 min and was validated per ICH and USP <1225> guidelines, demonstrating specificity, linearity, precision, accuracy, robustness, and reliable relative response factors. Overall, the AQbD framework enabled the development of a robust method suitable for determining these analytes in a variety of dietary ingredients derived from Mate and Guayusa leaves.
Source: ACS Omega
Institution: United States Pharmacopeial Convention
Language: English
Subfield: Analytical Chemistry
Field: Chemistry
Domain: Physical Sciences
Open Access status: gold
Estimated APC paid: $1,935
OpenAlex ID: W7223094674