Document Type
Oral Presentation
Location
Oxford Conference Center
Event Website
https://oxfordicsb.org/
Start Date
20-4-2026 1:55 PM
End Date
20-4-2026 2:15 PM
Description
Mate (Ilex paraguariensis) and Guayusa (Ilex guayusa), both members of the Aquifoliaceae family, have traditionally been consumed as herbal teas in South America. Their leaves are rich in methylxanthines and hydroxycinnamoylquinic acids—quinic acid derivatives of caffeic and gregrferulic acids—which provide stimulant and antioxidant properties. These compounds make them valuable for use in health and energy beverages as well as dietary supplements. We applied the Analytical Quality-by-Design (AQbD) approach to develop a robust UHPLC method for simultaneous quantification of methylxanthines and hydroxycinnamoylquinic acids. The method and sample preparation were designed in alignment with USP General Chapter < 1220> Analytical Procedure Life Cycle and ICH Q14 guidelines Analytical Procedure Development, for Mate and Guayusa leaves and their derived dietary ingredients (aqueous and hydroalcoholic extracts). Critical Method Attributes (CMAs) were defined based on the analytical target profile, and Critical Method Parameters (CMPs) were selected to optimize sample preparation and chromatographic conditions. The influence of CMP levels on CMAs was evaluated through a Design of Experiment (DOE). The developed UHPLC method achieves separation of three methylxanthines and nine hydroxycinnamoylquinic acids within a 12-minute runtime. Method robustness was established within the defined knowledge space, and the Method Operable Design Region (MODR) was generated. Optimal conditions were confirmed experimentally. Validation was performed according to USP General Chapter < 1225> Validation of Compendial Methods. The validated method is suitable for determining the content of methylxanthines and hydroxycinnamoylquinic acids in various dietary ingredients derived from Mate and Guayusa leaves and will be used for the ID and Composition tests of this family of monographs.
Recommended Citation
Monagas, Maria; Jeelani, Salika; Winter, Greg; and Kouznetsova, Natalia, "Application of AQbD principles to build a Robust Compendial Analytical Method for the Quantification of Phytochemicals in Mate and Guayusa Leaf Dietary Ingredients" (2026). Oxford ICSB. 3.
https://egrove.olemiss.edu/icsb/2026_ICSB/Schedule/3
Publication Date
April 2026
Accessibility Status
Screen reader accessible, Searchable text
Included in
Application of AQbD principles to build a Robust Compendial Analytical Method for the Quantification of Phytochemicals in Mate and Guayusa Leaf Dietary Ingredients
Oxford Conference Center
Mate (Ilex paraguariensis) and Guayusa (Ilex guayusa), both members of the Aquifoliaceae family, have traditionally been consumed as herbal teas in South America. Their leaves are rich in methylxanthines and hydroxycinnamoylquinic acids—quinic acid derivatives of caffeic and gregrferulic acids—which provide stimulant and antioxidant properties. These compounds make them valuable for use in health and energy beverages as well as dietary supplements. We applied the Analytical Quality-by-Design (AQbD) approach to develop a robust UHPLC method for simultaneous quantification of methylxanthines and hydroxycinnamoylquinic acids. The method and sample preparation were designed in alignment with USP General Chapter < 1220> Analytical Procedure Life Cycle and ICH Q14 guidelines Analytical Procedure Development, for Mate and Guayusa leaves and their derived dietary ingredients (aqueous and hydroalcoholic extracts). Critical Method Attributes (CMAs) were defined based on the analytical target profile, and Critical Method Parameters (CMPs) were selected to optimize sample preparation and chromatographic conditions. The influence of CMP levels on CMAs was evaluated through a Design of Experiment (DOE). The developed UHPLC method achieves separation of three methylxanthines and nine hydroxycinnamoylquinic acids within a 12-minute runtime. Method robustness was established within the defined knowledge space, and the Method Operable Design Region (MODR) was generated. Optimal conditions were confirmed experimentally. Validation was performed according to USP General Chapter < 1225> Validation of Compendial Methods. The validated method is suitable for determining the content of methylxanthines and hydroxycinnamoylquinic acids in various dietary ingredients derived from Mate and Guayusa leaves and will be used for the ID and Composition tests of this family of monographs.
https://egrove.olemiss.edu/icsb/2026_ICSB/Schedule/3
Comments
Dr. Maria Monagas is a Principal Scientist at the Department of Dietary Supplements and Herbal Medicines of the United States Pharmacopeia (USP). She has a Ph.D in Food Science and Technology from the Autonomous University of Madrid (Spain) and a MSc in Industrial Fermentation Technology from Heriot-Watt University (Scotland, United Kingdom). Before joining USP, she was a tenured track Research Scientist at the Spanish Scientific Research Council (CSIC) in Madrid, Spain. At USP, Dr. Monagas is responsible for the development and review of USP monographs and General Chapters related to ingredients of botanical origin to be admitted into the Dietary Supplements section of the USP-NF publication and the Dietary Supplements Compendium (DSC). She serves as a liaison between industry and USP Expert Committee members, and helps plan and organize USP Expert Committee work assignments. She is also responsible for the new USP Expert Panel on Botanical Dietary Supplements and Herbal Medicines for the Pan-American region. Dr. Monagas has more than 20 years of experience in the analysis and characterization of botanical ingredients used in the production of dietary supplements; particularly in ingredients derived from plants rich in polyphenols. She has contributed to more than 70 scientific publications, including original articles, book chapters, and industrial patents.