TitleQuantification of Caffeoylquinic Acids and Triterpenes as Targeted Bioactive Compounds of in Extracts and Formulations by Liquid Chromatography Mass Spectrometry.
Publication TypeJournal Article
Year of Publication2023
AuthorsYang L, Marney L, Magana AAlcazar, Choi J, Wright K, Mcferrin J, Gray NE, Soumyanath A, Stevens JF, Maier CS
JournalJ Chromatogr Open
Date Published2023 Nov 27

(CA) is a culinary vegetable and well-known functional food that is widely used as a medicinal herb and dietary supplement. CA is rich in pentacyclic triterpenes (TTs), including asiaticoside (AS), madecassoside (MS) and the related aglycones asiatic acid (AA), madecassic acid (MA). Traditionally, TTs have been associated with the bioactivity and health promoting effect of CA. Recently, mono-caffeoylquinic acids (MonoCQAs) and di-caffeoylquinic acids (DiCQAs) have been found to contribute to the bioactivity of CA as well. This work reports an analytical strategy based on liquid chromatography coupled to multiple reaction monitoring mass spectrometry (LC-MRM-MS) for the simultaneous rapid and accurate quantification of 12 bioactive compounds in CA, namely AS, MS, AA, MA, 5-CQA, 4-CQA, 3-CQA, 1,3-DiCQA, 3,4-DiCQA, 1,5-DiCQA, 3,5-DiCQA, 4,5-DiCQA. Method selectivity, accuracy, precision, repeatability, robustness, linearity range, limit of detection (LOD), and limit of quantitation (LOQ) were validated. The validated LC-MRM-MS method has been successfully applied to quantify the 12 bioactive compounds in CA aqueous extracts and two related formulations: a standardized CA product (CAP) used in a phase I clinical trial and formulated CA rodent diets used in preclinical studies. The validated method allows us to support the standardization of CA products used for clinical trials and conduct routine LC-MRM-MS analyses of formulated preclinical diets to confirm correct levels of CA phytochemical markers.

Alternate JournalJ Chromatogr Open
PubMed ID37789901
PubMed Central IDPMC10544816
Grant ListR61 AT009628 / AT / NCCIH NIH HHS / United States
S10 OD026922 / OD / NIH HHS / United States
T32 AT002688 / AT / NCCIH NIH HHS / United States
U19 AT010829 / AT / NCCIH NIH HHS / United States