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However, methods for their direct mass spectrometric detection in vivo remain underdeveloped, limiting the simultaneous analysis of their tissue distribution and associated metabolic responses. In this study, we developed a perylene-3,4,9,10-tetracarboxylic acid (PTCA)-labeling strategy for polystyrene (PS) nanospheres and established a direct laser desorption\/ionization mass spectrometry imaging (LDI-MSI) approach for in vivo tracking. On the same tissue section, PS\u2013PTCA was first imaged by LDI-MSI, followed by matrix application to obtain complementary metabolomic information. In an intravenous model, PS\u2013PTCA showed lung-dominant distribution and time-dependent metabolic responses, with acute purine perturbation followed by shifts in amino acid and nitrogen metabolism. Under an inhalation-relevant exposure setting established by intratracheal instillation, PS\u2013PTCA was confined to the lungs and persisted for weeks, accompanied by sustained metabolic alterations. This work provides a practical MSI framework for directly mapping in vivo PS biodistribution, together with associated metabolic responses.<\/jats:p>","DOI":"10.1021\/acs.analchem.6c03375","type":"journal-article","created":{"date-parts":[[2026,8,14]],"date-time":"2026-08-14T16:02:26Z","timestamp":1786723346000},"page":"24420-24429","source":"Crossref","is-referenced-by-count":0,"title":["A PTCA Labeling\nMethod for Direct LDI-MSI of Polystyrene\nNanospheres"],"prefix":"10.1021","volume":"98","author":[{"given":"Jinghan","family":"Fan","sequence":"first","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Beijing, China, 100190"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiameng","family":"Sun","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Beijing, China, 100190"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xi","family":"Yu","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Beijing, China, 100190"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8514-6348","authenticated-orcid":true,"given":"Zongxiu","family":"Nie","sequence":"additional","affiliation":[{"name":"Chinese Academy of Sciences , , ,","place":["Beijing, China, 100190"]},{"name":"University of Chinese Academy of Sciences , ,","place":["Beijing, China, 100049"]},{"name":"Hainan University , , ,","place":["Hainan, China, 570228"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,14]]},"reference":[{"issue":"6720","key":"2026083118461810100_cit1","doi-asserted-by":"publisher","DOI":"10.1126\/science.adl2746","article-title":"Twenty years of microplastic pollution research\u2500what\nhave we learned?","volume":"386","author":"Thompson","year":"2024","journal-title":"Science"},{"key":"2026083118461810100_cit2","doi-asserted-by":"publisher","DOI":"10.1016\/j.envint.2022.107199","article-title":"Discovery and quantification of plastic particle pollution\nin human blood","volume":"163","author":"Leslie","year":"2022","journal-title":"Environ. 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