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Acid hydrolysis using methanolysis is one adopted method of deconjugation that efficiently and rapidly cleaves both sulphates and glucuronides contemporaneously. The formation of artefactual by\u2010products is a known disadvantage of this harsh method. However, the possible promotion of deuterium\u2010hydrogen exchange of isotopically labelled internal standards has received little attention in the literature. This report demonstrates a complete deuterium\u2010hydrogen exchange from deuterium labelled D<jats:sub>9<\/jats:sub>\u2010progesterone to progesterone driven by the acidic conditions of the methanolysis. The likely mechanisms of this exchange reaction are postulated, and the results compared to other deuterated steroids. This finding highlights the importance for careful consideration when selecting labelled internal standards in a conjunction with methanolysis.<\/jats:p>","DOI":"10.1002\/dta.2402","type":"journal-article","created":{"date-parts":[[2018,5,14]],"date-time":"2018-05-14T10:46:30Z","timestamp":1526294790000},"page":"1469-1473","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["Important considerations for the utilisation of methanolysis in steroid analysis"],"prefix":"10.1002","volume":"10","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-7675-9812","authenticated-orcid":false,"given":"Marjaana","family":"Viljanto","sequence":"first","affiliation":[{"name":"LGC, Fordham  Cambridgeshire UK"},{"name":"Drug Control Centre, Analytical and Environmental Sciences Research Division, King's College London  UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Catarina Horro","family":"Pita","sequence":"additional","affiliation":[{"name":"LGC, Fordham  Cambridgeshire UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"James","family":"Scarth","sequence":"additional","affiliation":[{"name":"LGC, Fordham  Cambridgeshire UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Christopher J.","family":"Walker","sequence":"additional","affiliation":[{"name":"Drug Control Centre, Analytical and Environmental Sciences Research Division, King's College London  UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Andrew T.","family":"Kicman","sequence":"additional","affiliation":[{"name":"Drug Control Centre, Analytical and Environmental Sciences Research Division, King's College London  UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Mark C.","family":"Parkin","sequence":"additional","affiliation":[{"name":"Drug Control Centre, Analytical and Environmental Sciences Research Division, King's College London  UK"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2018,6,14]]},"reference":[{"key":"e_1_2_5_2_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jpba.2009.01.027"},{"key":"e_1_2_5_3_1","doi-asserted-by":"publisher","DOI":"10.1023\/b135931_9"},{"key":"e_1_2_5_4_1","unstructured":"WADA (World Anti\u2010Doping Agency).WADA Technical Document \u2010 TD2014EAAS\u2010 Endogenous anabolic androgenic steroids \u2010 Measurement and reporting.https:\/\/www.wada\u2010ama.org\/sites\/default\/files\/resources\/files\/wada\u2010td2014eaas\u2010v2\u2010endogenous\u2010anabolic\u2010androgenic\u2010steroids\u2010measurement\u2010and\u2010reporting\u2010en_0.pdf. 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