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However, their complicated preparation and associated expense limit broader application. In this study, novel magnetic particles with abundant N\u2010hydroxysuccinimide (NHS) esters on the surface are conveniently synthesized using a one\u2010pot method without carbodiimide activation carboxylate molecules. Subsequently, multifunctional probes are synthesized by immobilizing high\u2010density chemical probes on the surface of the magnetic materials through a postsynthetic modification strategy. This versatile probe facilitates the rapid capture of carboxylated compounds from complex matrices, with the labeled metabolites release from the magnetic materials subsequently analyzed using ultra\u2010high performance liquid chromatography\u2010mass spectrometry (UHPLC\u2010MS). The advantages of this innovative chemical biological tool include the simplicity and low cost of the synthesis, as well as the capability to analyze polar and volatile carboxylated metabolites via LC\u2010MS. This new strategy is successfully applied to analyze short\u2010chain fatty acids (SCFAs) in rat cecal contents, demonstrating the reliability of the analytical method. This study presents a cost\u2010effective and easy\u2010to\u2010implement approach for preparing NHS\u2010activated magnetic particles and offers a versatile probe with chemoselective extraction and labeling capabilities, providing a practical tool for analyzing SCFAs in the gut.<\/jats:p>","DOI":"10.1002\/advs.202413830","type":"journal-article","created":{"date-parts":[[2025,2,11]],"date-time":"2025-02-11T10:57:15Z","timestamp":1739271435000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["One\u2010Pot Construction of NHS\u2010Activated Magnetic Particles for Chemoselective Capture of Carboxyl Metabolites"],"prefix":"10.1002","volume":"12","author":[{"given":"Shuai","family":"Liu","sequence":"first","affiliation":[{"name":"State Key Laboratory of Bioactive Substance and Function of Natural Medicines Institute of Medicinal Plant Development Chinese Academy of Medical Sciences &amp; Peking Union Medical College 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