{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2025,10,10]],"date-time":"2025-10-10T01:59:45Z","timestamp":1760061585475,"version":"build-2065373602"},"reference-count":26,"publisher":"Wiley","issue":"3","license":[{"start":{"date-parts":[[2023,12,10]],"date-time":"2023-12-10T00:00:00Z","timestamp":1702166400000},"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":["Biomedical Chromatography"],"published-print":{"date-parts":[[2024,3]]},"abstract":"<jats:title>Abstract<\/jats:title><jats:p>In the present study, the main objective is to develop an analytical method for ultra\u2010trace level measurement of 2,6\u2010diamino\u20105\u2010nitropyrimidin\u20104(3H)\u2010one (DMNP) in valganciclovir hydrochloride (VAL) using liquid chromatography\u2010quadrupole time\u2010of\u2010flight\u2010tandem mass spectroscopy (LC\u2013QTOF\u2013MS\/MS). In the early stages of guanine synthesis, DMNP is formed, and guanine is known to be the key starting material for the synthesis of VAL. Taking into consideration DMNP potential genotoxicity, this analytical method has been developed. This method is time saving and suitable for confirming the masses of parent and fragment ions by MS and MS\/MS further fragmentation. An isocratic program and Acquity UPLC HSS cyano column (100\u2009\u00d7\u00a02.1\u00a0mm\u2009\u00d7\u00a01.8\u00a0\u03bcm) were used to achieve optimal separation between VAL and the DMNP impurity. A 0.1% ammonia solution in Milli\u2010Q water was used as mobile phase A, and methanol was used as mobile phase B in the ratio 90:10\u00a0v\/v in isocratic mode. In accordance with the International Conference on Harmonization's requirements, the developed method was validated. The detection and quantification levels were found to be 0.028 and 0.083\u2009ppm respectively. The DMNP impurity is linear from 0.083 to 1.245\u2009ppm levels with correlation coefficient (<jats:italic>R<\/jats:italic><jats:sup>2<\/jats:sup>) of 0.9960. The recoveries were found to be 97.0\u2013107.9%.<\/jats:p>","DOI":"10.1002\/bmc.5805","type":"journal-article","created":{"date-parts":[[2023,12,10]],"date-time":"2023-12-10T18:54:15Z","timestamp":1702234455000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":6,"title":["A novel liquid chromatography with quadrupole time\u2010of\u2010flight\u2010tandem mass spectroscopy method for ultra\u2010trace level identification and quantification of the genotoxic impurity 2,6\u2010diamino\u20105\u2010nitropyrimidin\u20104(3H)\u2010one in valganciclovir hydrochloride"],"prefix":"10.1002","volume":"38","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-9170-1352","authenticated-orcid":false,"given":"Shaik Mahammad","family":"Ali","sequence":"first","affiliation":[{"name":"Department of Chemistry Jawaharlal Nehru Technological University Anantapur  Ananthapuramu Andhra Pradesh India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6465-5696","authenticated-orcid":false,"given":"Manchuri Krishna","family":"Moorthy","sequence":"additional","affiliation":[{"name":"Department of Chemistry Jawaharlal Nehru Technological University Anantapur  Ananthapuramu Andhra Pradesh India"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Nayakanti","family":"Devanna","sequence":"additional","affiliation":[{"name":"Department of Chemistry JNTUA College of Engineering  Kalikiri, Annamayya District Andhra Pradesh India"}],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"311","published-online":{"date-parts":[[2023,12,10]]},"reference":[{"key":"e_1_2_7_2_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.pharma.2021.01.010"},{"key":"e_1_2_7_3_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jchromb.2011.09.041"},{"key":"e_1_2_7_4_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.toxlet.2004.04.004"},{"key":"e_1_2_7_5_1","doi-asserted-by":"publisher","DOI":"10.1365\/s10337-007-0259-x"},{"key":"e_1_2_7_6_1","doi-asserted-by":"publisher","DOI":"10.1515\/revac-2016-0025"},{"key":"e_1_2_7_7_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jchromb.2010.12.033"},{"key":"e_1_2_7_8_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.addr.2006.10.007"},{"key":"e_1_2_7_9_1","first-page":"1","article-title":"New UV spectrophotometric method for development and validation of valganciclovir hydrochloride in bulk and pharmaecutical dosage forms","volume":"7","author":"Karthik K.","year":"2020","journal-title":"IJCPA"},{"key":"e_1_2_7_10_1","first-page":"4773","article-title":"Development and validation of new spectroscopic method for the estimation of valganciclovir HCl in bulk and pharmaceutic dosage form","volume":"3","author":"Kumar K. 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