{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,9,24]],"date-time":"2026-09-24T23:13:57Z","timestamp":1790291637326,"version":"4.1.0"},"reference-count":13,"publisher":"Wiley","issue":"6","license":[{"start":{"date-parts":[[2025,5,5]],"date-time":"2025-05-05T00:00:00Z","timestamp":1746403200000},"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":[[2025,6]]},"abstract":"<jats:title>ABSTRACT<\/jats:title><jats:p>The high\u2010sensitivity analytical method for the detection of <jats:italic>N<\/jats:italic>\u2010nitroso duloxetine, which can be carcinogenic in duloxetine medication products, was successfully developed by applying liquid chromatography\u2013tandem mass spectrometry. Chromatographic separation was achieved by using liquid chromatography\u2013mass spectrometry was carried out by employing an Agilent Zorbax Eclipse Plus C18, 4.6\u2009\u00d7\u2009150\u2009mm, 5\u2010\u03bcm column. The gradient elution mode was used to operate the mobile phase, which consisted of Phase A, which was a solution of 0.1% ammonia and 0.1% formic acid in water, and Phase B, 100% methanol. This approach overcame duloxetine challenges. Tandem mass spectrometric detection with positive electro spray ionization in MRM mode then found <jats:italic>N<\/jats:italic>\u2010nitroso duloxetine. Quality control involves verifying the method for precision, specificity, linearity, accuracy, and robustness, following ICH and USP criteria &lt;1225&gt; to ensure suitability and consistent results. On the other hand, the correlation coefficient (<jats:italic>r<\/jats:italic>) was more than 1.000, the mean impurity recovery ranged from 100.5% to 102.4%, and the relative standard deviation (RSD) values (<jats:italic>n<\/jats:italic>\u2009=\u20096) ranged from 1.54% to 2.6% over the ranges of LOQ\u2014150%. This work seeks to simplify risk assessment for <jats:italic>N<\/jats:italic>\u2010nitroso duloxetine in duloxetine pharmaceutical formulations by providing a fast and reliable quantitative LC\u2010MS\/MS analytical method.<\/jats:p>","DOI":"10.1002\/bmc.70101","type":"journal-article","created":{"date-parts":[[2025,5,5]],"date-time":"2025-05-05T20:39:41Z","timestamp":1746477581000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":16,"title":["High\u2010Sensitivity LC\u2010MS\/MS Approach for Accurate Quantification of <i>N<\/i>\u2010Nitroso Duloxetine in Duloxetine Pharmaceutical Formulations"],"prefix":"10.1002","volume":"39","author":[{"ORCID":"https:\/\/orcid.org\/0009-0001-6171-8046","authenticated-orcid":false,"given":"Syam\u00a0Sundhar\u00a0Sai\u00a0Kumar","family":"Boppana","sequence":"first","affiliation":[{"name":"Vibrant Life Sciences Pvt Ltd.  Hyderabad Telangana India"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0002-8753-9713","authenticated-orcid":false,"given":"Kiran\u00a0Kumar","family":"Chagarlamudi","sequence":"additional","affiliation":[{"name":"Department of Chemistry Vignan's Foundation for Science Technology &amp; Research  Guntur Andhra Pradesh India"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0005-3665-9039","authenticated-orcid":false,"given":"Rajesh","family":"Damarapurapu","sequence":"additional","affiliation":[{"name":"CIS Pharma, APIIC Industrial Park  Nellore District Andhra Pradesh India"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0009-2555-8637","authenticated-orcid":false,"given":"Venkata\u00a0Siva\u00a0Suryanarayana","family":"Gurram","sequence":"additional","affiliation":[{"name":"CIS Pharma, APIIC Industrial Park  Nellore District Andhra Pradesh India"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0002-9384-292X","authenticated-orcid":false,"given":"Vinod\u00a0Kumar","family":"Manglige","sequence":"additional","affiliation":[{"name":"Vibrant Life Sciences Pvt Ltd.  Hyderabad Telangana India"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,5,5]]},"reference":[{"key":"e_1_2_8_2_1","unstructured":"EMAGuidelines: EMA\/409815\/2020 Rev.18; Question number\u201022 Effective from 02\u201010\u20102023."},{"key":"e_1_2_8_3_1","unstructured":"European Medicines Agency (EMA). \"Nitrosamine Impurities in Human Medicinal Products. FDA Guidance document on Recommended Acceptable Intake Limits for Nitrosamine Drug Substance\u2010Related Impurities Docket Number: FDA\u20102020\u2010D\u20101530 04 Aug(2023)."},{"key":"e_1_2_8_4_1","doi-asserted-by":"publisher","DOI":"10.1021\/acsomega.4c00136"},{"key":"e_1_2_8_5_1","unstructured":"ICH.2003.Stability Testing of New Drug Substances and Products Q1A (R2) Current Step 4 Version Dated 6 February 2003.https:\/\/database.ich.org\/sites\/default\/files\/Q1A%28R2%29%20Guideline.pdf."},{"key":"e_1_2_8_6_1","unstructured":"ICH.2005.Validation of Analytical Procedures: Text and Methodology Q2 (R1) Current Step 4 Version Dated 1996 and 2005.https:\/\/database.ich.org\/sites\/default\/files\/Q2%28R1%29%20Guideline.pdf."},{"key":"e_1_2_8_7_1","volume-title":"Validation of Analytical Procedures: Text and Methodology","author":"ICH Q2 (R2)","year":"2022"},{"key":"e_1_2_8_8_1","doi-asserted-by":"publisher","DOI":"10.31788\/RJC.2020.1335819"},{"key":"e_1_2_8_9_1","doi-asserted-by":"publisher","DOI":"10.1186\/s40543\u2010021\u201000273\u20107"},{"key":"e_1_2_8_10_1","doi-asserted-by":"publisher","DOI":"10.1007\/s13738\u2010020\u201002118\u20103"},{"key":"e_1_2_8_11_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.pharma.2022.06.010"},{"key":"e_1_2_8_12_1","unstructured":"National Center for Biotechnology Information.2025.PubChem Compound Summary for CID 60835 Duloxetine. Retrieved January 26 2025 fromhttps:\/\/pubchem.ncbi.nlm.nih.gov\/compound\/Duloxetine."},{"key":"e_1_2_8_13_1","doi-asserted-by":"publisher","DOI":"10.14233\/ajchem.2023.30576"},{"key":"e_1_2_8_14_1","volume-title":"<1225> Validation of Compendial Procedures","author":"United States Pharmacopeia (USP)","year":"2020"}],"container-title":["Biomedical Chromatography"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/analyticalsciencejournals.onlinelibrary.wiley.com\/doi\/pdf\/10.1002\/bmc.70101","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,9]],"date-time":"2025-10-09T22:00:50Z","timestamp":1760047250000},"score":1,"resource":{"primary":{"URL":"https:\/\/analyticalsciencejournals.onlinelibrary.wiley.com\/doi\/10.1002\/bmc.70101"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2025,5,5]]},"references-count":13,"journal-issue":{"issue":"6","published-print":{"date-parts":[[2025,6]]}},"alternative-id":["10.1002\/bmc.70101"],"URL":"https:\/\/doi.org\/10.1002\/bmc.70101","archive":["Portico"],"relation":{},"ISSN":["0269-3879","1099-0801"],"issn-type":[{"value":"0269-3879","type":"print"},{"value":"1099-0801","type":"electronic"}],"subject":[],"published":{"date-parts":[[2025,5,5]]},"assertion":[{"value":"2025-03-19","order":0,"name":"received","label":"Received","group":{"name":"publication_history","label":"Publication History"}},{"value":"2025-04-23","order":2,"name":"accepted","label":"Accepted","group":{"name":"publication_history","label":"Publication History"}},{"value":"2025-05-05","order":3,"name":"published","label":"Published","group":{"name":"publication_history","label":"Publication History"}}],"article-number":"e70101"}}