Amphipterygium adstringens (cuachalalate) is a medicinal plant widely used in traditional Mexican medicine for its anti-inflammatory, gastroprotective, and antimicrobial properties. In this study, we applied qualitative and quantitative NMR-based metabolomics profiling, combined with multivariate statistical analyses, including Principal Component Analysis (PCA), Partial Least Squares Discriminant Analysis (PLS-DA), and S-plots, to evaluate the chemical composition and authenticity of A. adstringens samples collected from different commercial sources sold in Mexico City. Metabolomic profiles in organic and aqueous extracts revealed highly similar spectral patterns among all collected samples, supporting the consistency of commercially available A. adstringens in Mexico. The presence of 3α-hydroxy-masticadienoic acid (3α-HMDA) and anacardic acids, biomarkers of the genus, was confirmed by ¹H NMR in hexane extracts; in the aqueous extract they were not observed with the same analytical platform. These findings suggest that the traditional infusion method may not effectively extract the above-mentioned key bioactive compounds. This approach enhances quality control and ensures the reliability of A. adstringens products in the commercial market.

Aqueous extracts of seven commercial samples of boldo leaves (Peumus boldus) were subjected to 1H NMR analysis to elucidate their chemical profiling. The ground leaves were extracted with ultrasound using water as a solvent at 60 °C for 15 min. The resulting extracts were then analyzed using 1H NMR spectroscopy, unveiling the presence of seven amino acids (alanine, asparagine, glutamine, phenylalanine, proline, tyrosine, and valine), three sugars (α- and β-glucose, fructose, and sucrose), and seven short-chain carboxylic acids (acetic, citric, formic, glyceric, malic, malonic, and succinic acids). Through multivariate statistical analysis of the gathered 1H NMR data, including PCA and OPLS-DA, a consistent chemical profile emerged across the examined samples. Variations were mainly due to differences in the relative concentrations of the mentioned metabolites. In addition, High Resolution Mass Spectrometry-ESI (HRMS-ESI) confirmed the presence of boldine in all samples tested, aiding in the authentication of boldo samples. Additionally, the major alkaloid N-methyllaurotetanine, a typical component of boldo leaves, was also identified. Resumen. Los extractos acuosos de siete muestras comerciales de hojas de boldo (Peumus boldus) se sometieron a análisis de RMN 1H para dilucidar su perfil químico. Las hojas molidas se extrajeron por ultrasonido utilizando agua como disolvente a 60°C durante 15 minutos. Los extractos resultantes se sometieron a análisis por RMN 1H, revelando la presencia de siete aminoácidos (alanina, asparagina, glutamina, fenilalanina, prolina, tirosina y valina), tres azúcares (α y β-glucosa, fructosa y sacarosa) y siete ácidos carboxílicos de cadena corta (acético, cítrico, glicérico, málico, malónico y succínico). Mediante el análisis estadístico multivariante de los datos de RMN 1H reunidos, incluyendo PCA y OPLS-DA, se observó un perfil químico coherente en todas las muestras examinadas. Las variaciones se debieron principalmente a diferencias en las concentraciones relativas de los metabolitos mencionados. Además, la espectrometría de masas de alta resolución-ESI (HRMS-ESI) confirmó la presencia de boldina en todas las muestras analizadas, ayudando a la autenticación de las muestras de boldo. También se identificó el alcaloide principal N-metillaurotetanina, un componente típico de las hojas de boldo.

This study aimed to characterize the metabolomic profile of aqueous extracts of Hypericum perforatum (St. John’s wort) commercial samples using ¹H NMR spectroscopy, in order to evaluate their chemical composition as consumed in infusion form. Seven retail samples were extracted with water under conditions simulating tea preparation and analyzed using ¹H NMR. Metabolite identification and quantification were performed with Chenomx^® software, followed by multivariate statistical analyses including PCA and OPLS-DA. A total of 37 metabolites were identified, predominantly primary metabolites such as sugars (glucose, fructose), amino acids (glycine, asparagine), short-chain organic acids (malic, citric, and acetic acids), secondary metabolites (trigonelline, chlorogenic acid) and metabolism products (methanol, ethanol, acetic acid and acetone). Notably, key bioactive compounds traditionally associated with H. perforatum, such as hypericin and hyperforin, were not detected under the experimental conditions employed. Multivariate analyses revealed significant variability among samples, suggesting differences in composition likely related to origin, processing, or potential adulteration. These findings demonstrate that aqueous preparations of St. John’s wort differ substantially from extracts used in clinical trials, being dominated by primary metabolism rather than specialized bioactive compounds. This has important implications for the interpretation of its therapeutic effects when consumed as tea. Furthermore, the study highlights the utility of NMR-based metabolomics as a robust tool for quality assessment and authentication of herbal products.