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Even though colistin has been used for more than 50 years, its metabolic fate is poorly understood. One of the current challenges for studying the pharmacokinetics (PK) is the precise and accurate determination of colistin in <jats:italic>in vitro<\/jats:italic> and <jats:italic>in vivo<\/jats:italic> studies. In the present study, we developed and validated a series of sensitive and robust liquid chromatography tandem mass spectrometry (LC\u2013MS\/MS) methods for analysing biological samples obtained from <jats:italic>in vitro<\/jats:italic> and in <jats:italic>vivo<\/jats:italic> disposition assays. After a zinc acetate\u2010mediated precipitation, hydrophilic\u2013lipophilic\u2010balanced solid phase extraction (HLB\u2010SPE) was used for the extraction of colistin. The compounds were retained on a hydrophilic interaction liquid chromatography (HILIC) column and were detected by MS\/MS. CMS was quantified by determining the produced amount of colistin during acidic hydrolysis. The developed methods are sensitive with lower limits of quantification varying between 0.009 \u03bcg\/mL and 0.071 \u03bcg\/mL for colistin A, and 0.002 \u03bcg\/mL to 0.013 \u03bcg\/mL for colistin B. The intra\u2010 and inter\u2010day precision and accuracy were within \u00b115%. Calibration curves of colistin were linear (0.063 \u03bcg\/mL to 8.00 \u03bcg\/mL) within clinically relevant concentration ranges. Zinc acetate\u2010mediated precipitation and the use of a HILIC column were found to be essential. The developed methods are sensitive, accurate, precise, highly efficient and allow monitoring colistin and CMS in biological samples without the need for an internal standard.<\/jats:p>","DOI":"10.1002\/dta.2812","type":"journal-article","created":{"date-parts":[[2020,4,26]],"date-time":"2020-04-26T01:19:55Z","timestamp":1587863995000},"page":"1183-1195","update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":24,"title":["Quantitative determination of colistin A\/B and colistin methanesulfonate in biological samples using hydrophilic interaction chromatography tandem mass spectrometry"],"prefix":"10.1002","volume":"12","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-8025-493X","authenticated-orcid":false,"given":"Bing","family":"Qi","sequence":"first","affiliation":[{"name":"Drug Delivery and Disposition KU Leuven Department of Pharmaceutical and Pharmacological Sciences  Leuven 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