{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,9,9]],"date-time":"2026-09-09T19:35:40Z","timestamp":1788982540816,"version":"build-2803163510"},"reference-count":47,"publisher":"MDPI AG","issue":"16","license":[{"start":{"date-parts":[[2025,8,14]],"date-time":"2025-08-14T00:00:00Z","timestamp":1755129600000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"name":"Natural Health Product Research Alliance, University of Guelph","award":["053312"],"award-info":[{"award-number":["053312"]}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Molecules"],"abstract":"<jats:p>Metabolite fingerprint profiling is a robust tool for verifying suppliers of authentic botanical ingredients. While comparative studies exist, few apply identical conditions across multiple species; this study utilized a cross-species comparison to identify versatile solvents despite biochemical variability. Multiple solvents were used for sample extraction prior to analysis by proton NMR and liquid chromatography\u2013mass spectrometry (LC-MS) for multiple botanicals including Camellia sinensis, Cannabis sativa, Myrciaria dubia, Sambucus nigra, Zingiber officinale, Curcuma longa, Silybum marianum, Vaccinium macrocarpon, and Prunus cerasus. Comparisons were normalized by total intensity; deuterated methanol aids NMR lock but is not required for LC-MS. Hierarchical clustering analysis (HCA) evaluated solvent efficacy. Methanol\u2013deuterium oxide (1:1) was the most effective extraction method, yielding 155 NMR spectral metabolite variables for Camellia sinensis, while methanol (90% CH3OH + 10% CD3OD) produced 198 for Cannabis sativa and 167 for Myrciaria dubia, with 11, 9, and 28 assigned metabolites, respectively. LC-MS detected 121 metabolites in Myrciaria dubia in methanol as the most effective extraction method. Methanol (10% deuterated) is the most effective extraction method for comprehensive metabolite fingerprinting using NMR and LC-MS protocols because it provides the broadest metabolite coverage. This study advances fit-for-purpose methods to qualify suppliers of botanical ingredients in food and NHP quality control programs.<\/jats:p>","DOI":"10.3390\/molecules30163379","type":"journal-article","created":{"date-parts":[[2025,8,14]],"date-time":"2025-08-14T15:16:37Z","timestamp":1755184597000},"page":"3379","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":8,"title":["Optimization of Extraction Methods for NMR and LC-MS Metabolite Fingerprint Profiling of Botanical Ingredients in Food and Natural Health Products (NHPs)"],"prefix":"10.3390","volume":"30","author":[{"ORCID":"https:\/\/orcid.org\/0009-0005-9226-447X","authenticated-orcid":false,"given":"Varathan","family":"Vinayagam","sequence":"first","affiliation":[{"name":"College of Biological Science, University of Guelph, Guelph, ON N1G 2W1, Canada"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7948-2257","authenticated-orcid":false,"given":"Arunachalam","family":"Thirugnanasambandam","sequence":"additional","affiliation":[{"name":"College of Biological Science, University of Guelph, Guelph, ON N1G 2W1, Canada"},{"name":"Biological and Life Sciences, Canadian Light Source, Saskatoon, SK S7N 2V3, Canada"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5181-005X","authenticated-orcid":false,"given":"Subramanyam","family":"Ragupathy","sequence":"additional","affiliation":[{"name":"College of Biological Science, University of Guelph, Guelph, ON N1G 2W1, Canada"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0001-1882-6287","authenticated-orcid":false,"given":"Ragupathy","family":"Sneha","sequence":"additional","affiliation":[{"name":"College of Biological Science, University of Guelph, Guelph, ON N1G 2W1, Canada"},{"name":"College of Medicine, American University of Antigua, Jobberwock Beach Road, Coolidge P.O. Box W1451, Antigua and Barbuda"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8707-7769","authenticated-orcid":false,"given":"Steven G.","family":"Newmaster","sequence":"additional","affiliation":[{"name":"College of Biological Science, University of Guelph, Guelph, ON N1G 2W1, Canada"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2025,8,14]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","unstructured":"Emwas, A.H., Roy, R., McKay, R.T., Tenori, L., Saccenti, E., Nagana Gowda, G.A., Raftery, D., Alahmari, F., Jaremko, L., and Jaremko, M. (2019). Nmr Spectroscopy for Metabolomics Research. Metabolites, 9.","DOI":"10.3390\/metabo9070123"},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"155","DOI":"10.1016\/j.jmr.2019.07.013","article-title":"NMR Metabolomics: A Look Ahead","volume":"306","author":"Wishart","year":"2019","journal-title":"J. Magn. 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