{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2025,10,29]],"date-time":"2025-10-29T06:24:41Z","timestamp":1761719081346,"version":"build-2065373602"},"reference-count":26,"publisher":"Wiley","issue":"2","license":[{"start":{"date-parts":[[2021,10,26]],"date-time":"2021-10-26T00:00:00Z","timestamp":1635206400000},"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":["Drug Testing and Analysis"],"published-print":{"date-parts":[[2022,2]]},"abstract":"<jats:title>Abstract<\/jats:title><jats:p>Prenylamine was initially used for the treatment of angina pectoris and later on withdrawn from the market in 1988 due to cardiac arrhythmias concern. The major phase I metabolite of prenylamine is <jats:italic>p<\/jats:italic>\u2010hydroxy prenylamine that has a chiral center in the structure. Even though <jats:italic>p<\/jats:italic>\u2010hydroxy prenylamine was synthesized earlier, it lacked complete analytical developments for chiral high\u2010performance liquid chromatography (HPLC) separation. However, <jats:italic>p<\/jats:italic>\u2010hydroxy prenylamine reference material is not commercially available. The innovation of this manuscript is the development and validation of a chiral HPLC separation method and more extensive characterization of the reference material than previously reported method. Therefore, it was hypothesized to develop and validate normal phase HPLC method for <jats:italic>p<\/jats:italic>\u2010hydroxy prenylamine reference material. <jats:italic>p<\/jats:italic>\u2010Hydroxy prenylamine was synthesized in two batches and characterized successfully using <jats:sup>13<\/jats:sup>C NMR, <jats:sup>1<\/jats:sup>H NMR, high\u2010resolution mass spectrometry (HRMS), Fourier transform infrared spectroscopy (FT\u2010IR), and thermogravimetric analysis (TGA). A normal phase chiral HPLC method was developed to analyze the <jats:italic>p<\/jats:italic>\u2010hydroxy prenylamine purity. Separation of the <jats:italic>p<\/jats:italic>\u2010hydroxy prenylamine enantiomers were achieved using ultra\u2010high\u2010performance liquid chromatography (UHPLC) on a ChiralCel ODH column at wavelength of 220\u2009nm. The developed method was validated in terms of its linearity, accuracy, precision, and robustness for purification, purity assessment, and stability studies. Proton and carbon peaks were confirmed by nuclear magnetic resonance (NMR) analysis. Functional groups were confirmed by FT\u2010IR. Loss on drying was 0.3% and 0.6% for Batches 1 and 2, respectively. The purity of the developed reference material for Batches 1 and 2 was found to be 99.59% and 100%, respectively. Therefore, the synthesized batches of <jats:italic>p<\/jats:italic>\u2010hydroxy prenylamine can be used in dope testing as reference material.<\/jats:p>","DOI":"10.1002\/dta.3171","type":"journal-article","created":{"date-parts":[[2021,10,8]],"date-time":"2021-10-08T20:15:55Z","timestamp":1633724155000},"page":"224-232","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":11,"title":["Analytical developments of <i>p<\/i>\u2010hydroxy prenylamine reference material for dope control research: Characterization and purity assessment"],"prefix":"10.1002","volume":"14","author":[{"given":"Athira","family":"Joseph","sequence":"first","affiliation":[{"name":"Department of Pharmaceutical Analysis National Institute of Pharmaceutical Education and Research (NIPER)  SilaKatamur (Halugurisuk), P.O.: Changsari, Dist: Kamrup Guwahati Assam 781101 India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Gangasani Jagadeesh","family":"Kumar","sequence":"additional","affiliation":[{"name":"Department of Pharmaceutical Analysis National Institute of Pharmaceutical Education and Research (NIPER)  SilaKatamur (Halugurisuk), P.O.: Changsari, Dist: Kamrup Guwahati Assam 781101 India"},{"name":"Department of Medicinal Chemistry National Institute of Pharmaceutical Education and Research (NIPER)  SilaKatamur (Halugurisuk), P.O.: Changsari, Dist: Kamrup Guwahati Assam 781101 India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9085-029X","authenticated-orcid":false,"given":"Sachin Dattram","family":"Pawar","sequence":"additional","affiliation":[{"name":"Department of Pharmaceutical Analysis National Institute of Pharmaceutical Education and Research (NIPER)  SilaKatamur (Halugurisuk), P.O.: Changsari, Dist: Kamrup Guwahati Assam 781101 India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Bhakti Umesh","family":"Hirlekar","sequence":"additional","affiliation":[{"name":"Department of Medicinal Chemistry National Institute of Pharmaceutical Education and Research (NIPER)  SilaKatamur (Halugurisuk), P.O.: Changsari, Dist: Kamrup Guwahati Assam 781101 India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Prasad V.","family":"Bharatam","sequence":"additional","affiliation":[{"name":"Department of Medicinal Chemistry National Institute of Pharmaceutical Education and Research (NIPER)  Sector 67, S.A.S. 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L.","family":"Sahu","sequence":"additional","affiliation":[{"name":"National Dope Testing Laboratory  J.L.N Stadium Complex, East Gate No. 10, Near MTNL Building New Delhi 110003 India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Sachin","family":"Dubey","sequence":"additional","affiliation":[{"name":"National Dope Testing Laboratory  J.L.N Stadium Complex, East Gate No. 10, Near MTNL Building New Delhi 110003 India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"P.","family":"Radhakrishnanand","sequence":"additional","affiliation":[{"name":"Department of Pharmaceutical Analysis National Institute of Pharmaceutical Education and Research (NIPER)  SilaKatamur (Halugurisuk), P.O.: Changsari, Dist: Kamrup Guwahati Assam 781101 India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Daya Raju","family":"Adye","sequence":"additional","affiliation":[{"name":"Department of Pharmaceutical Analysis National Institute of Pharmaceutical 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