{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,5,16]],"date-time":"2026-05-16T03:49:12Z","timestamp":1778903352345,"version":"3.51.4"},"reference-count":22,"publisher":"Wiley","issue":"22","license":[{"start":{"date-parts":[[2024,9,6]],"date-time":"2024-09-06T00:00:00Z","timestamp":1725580800000},"content-version":"vor","delay-in-days":0,"URL":"http:\/\/onlinelibrary.wiley.com\/termsAndConditions#vor"}],"content-domain":{"domain":["analyticalsciencejournals.onlinelibrary.wiley.com"],"crossmark-restriction":true},"short-container-title":["Rapid Comm Mass Spectrometry"],"published-print":{"date-parts":[[2024,11,30]]},"abstract":"<jats:p>In the mirabegron (MIR) synthesis, the N\u2010nitroso mirabegron (NNM) is obtained during synthetic process of MIR; water is being used in reaction under acidic condition. Nitrite source is from water, and secondary amine source is from MIR as it has secondary amine; NNM is generated as an impurity during the synthesis of MIR. The presence of NNM in MIR could potentially affect its effectiveness. The purpose of this study was to establish a Ultra\u2010performance liquid chromatography\u2010mass spectrometry\/mass spectrometry\u00a0(UPLC\u2010MS\/MS)\u00a0methodology to identify NNM in MIR samples. The method for NNM analysis was developed on Acquity HSS T3 (100*2.1) mm 1.8\u00a0\u03bcm column with gradient elution using mobile phase consisted of 0.1% formic acid in water (mobile phase A) and 0.1% formic acid in methanol (mobile phase B). Mass spectrometer with electrospray ionization operated in the MRM mode was used in the analysis of NNM (m\/ z 426.20\u2009\u2192\u2009170.00). The UPLC\u2010MS\/MS methodology proposed showed a good linearity (0.02 to 0.72\u2009ppm), good system precision (RSD\u2009=\u20090.57%), good method precision (RSD\u2009=\u20090.87%), acceptable accuracy (94.5\u2013116.5%), low detection limit (0.006\u2009ppm) and low quantification limit (0.02\u2009ppm) for NNM. The UPLC\u2010MS\/MS methodology proposed can be utilized to assess the quality of MIR sample for the presence of NNM impurity.<\/jats:p>","DOI":"10.1002\/rcm.9911","type":"journal-article","created":{"date-parts":[[2024,9,6]],"date-time":"2024-09-06T03:13:47Z","timestamp":1725592427000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Development of an UPLC\u2010MS\/MS approach to detect and quantify N\u2010nitroso mirabegron in mirabegron"],"prefix":"10.1002","volume":"38","author":[{"given":"Ravi","family":"Uppala","sequence":"first","affiliation":[{"name":"Department of Chemistry Faculty of Engineering and Technology, SRM Institute of Science and Technology  India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8330-4883","authenticated-orcid":false,"given":"Rakesh Chandrakant","family":"Prabhu","sequence":"additional","affiliation":[{"name":"Department of Chemistry Faculty of Engineering and Technology, SRM Institute of Science and Technology  India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1794-3967","authenticated-orcid":false,"given":"Arthanareeswari","family":"Maruthapillai","sequence":"additional","affiliation":[{"name":"Department of Chemistry Faculty of Engineering and Technology, SRM Institute of Science and Technology  India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Bandaru","family":"Venkatasubbaiah","sequence":"additional","affiliation":[{"name":"Dr. Reddys IPDO  Hyderabad India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0149-5423","authenticated-orcid":false,"given":"Gopal Chandru","family":"Senadi","sequence":"additional","affiliation":[{"name":"Department of Chemistry Faculty of Engineering and Technology, SRM Institute of Science and Technology  India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1224-0947","authenticated-orcid":false,"given":"Sundaramurthy","family":"Devikala","sequence":"additional","affiliation":[{"name":"Department of Chemistry Faculty of Engineering and Technology, SRM Institute of Science and Technology  India"}],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"311","published-online":{"date-parts":[[2024,9,6]]},"reference":[{"key":"e_1_2_9_2_1","unstructured":"MIRMonograph for Professionals. 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Retrieved 7 October 2022 https:\/\/clincalc.com\/DrugStats\/Top300Drugs.aspx"},{"key":"e_1_2_9_9_1","unstructured":"MIR\u2010 Drug Usage Statistics.ClinCalc. Retrieved 7 October 2022 https:\/\/clincalc.com\/DrugStats\/Drugs\/Mirabegron"},{"key":"e_1_2_9_10_1","unstructured":"2022 First Generic Drug Approvals.U.S. Food and Drug Administration (FDA). 3 March 2023. Archived from the original on 30 June 2023. 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