{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2025,10,11]],"date-time":"2025-10-11T00:09:16Z","timestamp":1760141356899,"version":"build-2065373602"},"reference-count":18,"publisher":"Wiley","issue":"12","license":[{"start":{"date-parts":[[2024,11,6]],"date-time":"2024-11-06T00:00:00Z","timestamp":1730851200000},"content-version":"vor","delay-in-days":0,"URL":"http:\/\/creativecommons.org\/licenses\/by-nc-nd\/4.0\/"}],"content-domain":{"domain":["analyticalsciencejournals.onlinelibrary.wiley.com"],"crossmark-restriction":true},"short-container-title":["Biomedical Chromatography"],"published-print":{"date-parts":[[2024,12]]},"abstract":"<jats:title>Abstract<\/jats:title><jats:p>Bedaquiline (BDQ) is a drug used to treat multidrug\u2010resistant tuberculosis (MDR\u2010TB). It exhibits exposure\u2010dependent efficacy in eliminating <jats:styled-content style=\"fixed-case\"><jats:italic>Mycobacterium tuberculosis<\/jats:italic><\/jats:styled-content> (Mtb). An easy, efficient and precise reverse\u2010phase ultrafast liquid chromatography (RP\u2010UFLC) method was developed to validate the free base of the antitubercular medication BDQ. BDQ was separated using a 10:90\u2009v\/v mobile phase of ammonium acetate buffer solution (pH\u2009=\u20095.4) and high\u2010performance liquid chromatography\u2013grade methanol, with a flow rate of 1.5\u00a0mL\/min and a UV detection wavelength of 226\u2009nm. By using the Box\u2013Behnken design (BBD) and response surface methodology (RSM), the method was optimised by varying critical analytical attributes (CAA) and critical performance attributes (CPAs) namely ammonium acetate fraction (%), flow rate (ml\/min), buffer system molarity (M) and pH. BDQ was eluted at 7.5\u00a0min utilising isocratic elution. The method was linear in the concentration range of 0.5\u2013300\u2009\u03bcg\/mL with limit of detection values of 0.039\u2009\u03bcg\/mL and limit of quantification of 0.12\u2009\u03bcg\/mL. The results indicate that this validated method can be used as an alternative method for assay of BDQ.<\/jats:p>","DOI":"10.1002\/bmc.6037","type":"journal-article","created":{"date-parts":[[2024,11,6]],"date-time":"2024-11-06T06:04:37Z","timestamp":1730873077000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Method development and validation of an analytical quality by design ultrafast liquid chromatographic method for the determination of bedaquiline from pharmaceutical bulk and nanoemulsions"],"prefix":"10.1002","volume":"38","author":[{"given":"Taiwo Oreoluwa","family":"Ajayi","sequence":"first","affiliation":[{"name":"Department of Pharmaceutical Sciences, School of Pharmacy Sefako Makgatho Health Sciences University  Pretoria South Africa"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Madan Sai","family":"Poka","sequence":"additional","affiliation":[{"name":"Department of Pharmaceutical Sciences, School of Pharmacy Sefako Makgatho Health Sciences University  Pretoria South Africa"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4034-9368","authenticated-orcid":false,"given":"Bwalya Angel","family":"Witika","sequence":"additional","affiliation":[{"name":"Department of Pharmaceutical Sciences, School of Pharmacy Sefako Makgatho Health Sciences University  Pretoria South Africa"}],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"311","published-online":{"date-parts":[[2024,11,6]]},"reference":[{"key":"e_1_2_5_2_1","doi-asserted-by":"publisher","DOI":"10.1128\/AAC.00276-15"},{"key":"e_1_2_5_3_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.talanta.2008.05.019"},{"key":"e_1_2_5_4_1","doi-asserted-by":"publisher","DOI":"10.1056\/nejmp1314385"},{"key":"e_1_2_5_5_1","doi-asserted-by":"publisher","DOI":"10.1093\/chromsci\/bmw050"},{"key":"e_1_2_5_6_1","doi-asserted-by":"publisher","DOI":"10.1111\/bcp.12613"},{"key":"e_1_2_5_7_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jpba.2019.07.023"},{"key":"e_1_2_5_8_1","doi-asserted-by":"publisher","DOI":"10.1186\/1471-2288-11-118"},{"key":"e_1_2_5_9_1","doi-asserted-by":"publisher","DOI":"10.1002\/chir.23037"},{"key":"e_1_2_5_10_1","unstructured":"Okezue M. Okezue M. A. &Byrn S. J..2022.Mechanisms for improving the clinical success of a low\u2010water soluble new drug moiety the bedaquiline case study."},{"key":"e_1_2_5_11_1","doi-asserted-by":"publisher","DOI":"10.1186\/s43094-020-00061-x"},{"key":"e_1_2_5_12_1","doi-asserted-by":"publisher","DOI":"10.1186\/s43094-021-00235-1"},{"key":"e_1_2_5_13_1","doi-asserted-by":"publisher","DOI":"10.2174\/1574891x12666170619101904"},{"key":"e_1_2_5_14_1","doi-asserted-by":"publisher","DOI":"10.4103\/2229-5186.79345"},{"issue":"1","key":"e_1_2_5_15_1","first-page":"26","article-title":"HPLC method development and validation\u2014An overview","volume":"4","author":"Singh R.","year":"2013","journal-title":"Journal of Pharmaceutical Education & Research"},{"key":"e_1_2_5_16_1","first-page":"11","article-title":"The diarylquinoline TMC207 for multidrug\u2010resistant tuberculosis","volume":"355","author":"Stein P. D.","year":"2006","journal-title":"New England Journal of Medicine"},{"key":"e_1_2_5_17_1","unstructured":"U.S. Department of Health and Human Services.2001.Food and Drug Administration. Guidance for industry: Bioanalytical method validation. Fda no. May 4\u201310."},{"key":"e_1_2_5_18_1","doi-asserted-by":"publisher","DOI":"10.1093\/chromsci\/bmab117"},{"key":"e_1_2_5_19_1","unstructured":"World Health Organization. (2022).Global tuberculosis report. 2022. 978 92 4 156450 2."}],"container-title":["Biomedical Chromatography"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/analyticalsciencejournals.onlinelibrary.wiley.com\/doi\/pdf\/10.1002\/bmc.6037","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,10]],"date-time":"2025-10-10T00:58:56Z","timestamp":1760057936000},"score":1,"resource":{"primary":{"URL":"https:\/\/analyticalsciencejournals.onlinelibrary.wiley.com\/doi\/10.1002\/bmc.6037"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2024,11,6]]},"references-count":18,"journal-issue":{"issue":"12","published-print":{"date-parts":[[2024,12]]}},"alternative-id":["10.1002\/bmc.6037"],"URL":"https:\/\/doi.org\/10.1002\/bmc.6037","archive":["Portico"],"relation":{},"ISSN":["0269-3879","1099-0801"],"issn-type":[{"type":"print","value":"0269-3879"},{"type":"electronic","value":"1099-0801"}],"subject":[],"published":{"date-parts":[[2024,11,6]]},"assertion":[{"value":"2024-06-27","order":0,"name":"received","label":"Received","group":{"name":"publication_history","label":"Publication History"}},{"value":"2024-10-23","order":2,"name":"accepted","label":"Accepted","group":{"name":"publication_history","label":"Publication History"}},{"value":"2024-11-06","order":3,"name":"published","label":"Published","group":{"name":"publication_history","label":"Publication History"}}],"article-number":"e6037"}}