{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,1,18]],"date-time":"2026-01-18T13:24:33Z","timestamp":1768742673304,"version":"3.49.0"},"reference-count":21,"publisher":"MDPI AG","issue":"6","license":[{"start":{"date-parts":[[2020,3,22]],"date-time":"2020-03-22T00:00:00Z","timestamp":1584835200000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"DOI":"10.13039\/501100001871","name":"Funda\u00e7\u00e3o para a Ci\u00eancia e a Tecnologia","doi-asserted-by":"publisher","award":["UIDB\/00100\/2020 ; UIDP\/00100\/2020 ; SFRH\/BD\/107892\/2015"],"award-info":[{"award-number":["UIDB\/00100\/2020 ; UIDP\/00100\/2020 ; SFRH\/BD\/107892\/2015"]}],"id":[{"id":"10.13039\/501100001871","id-type":"DOI","asserted-by":"publisher"}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Molecules"],"abstract":"<jats:p>We developed, optimized and validated a fast analytical cycle using high throughput bar adsorptive microextraction and microliquid desorption (HT-BA\u03bcE-\u03bcLD) for the extraction and desorption of ketamine and norketamine in up to 100 urine samples simultaneously, resulting in an assay time of only 0.45 min\/sample. The identification and quantification were carried out using large volume injection-gas chromatography-mass spectrometry operating in the selected ion monitoring mode (LVI-GC-MS(SIM)). Several parameters that could influencing HT-BA\u00b5E were assayed and optimized in order to maximize the recovery yields of ketamine and norketamine from aqueous media. These included sorbent selectivity, desorption solvent and time, as well as shaking rate, microextraction time, matrix pH, ionic strength and polarity. Under optimized experimental conditions, suitable sensitivity (1.0 \u03bcg L\u22121), accuracy (85.5\u2013112.1%), precision (\u226415%) and recovery yields (84.9\u2013105.0%) were achieved. Compared to existing methods, the herein described analytical cycle is much faster, environmentally friendly and cost-effective for the quantification of ketamine and norketamine in urine samples. To our knowledge, this is the first work that employs a high throughput based microextraction approach for the simultaneous extraction and subsequent desorption of ketamine and norketamine in up to 100 urine samples simultaneously.<\/jats:p>","DOI":"10.3390\/molecules25061438","type":"journal-article","created":{"date-parts":[[2020,4,3]],"date-time":"2020-04-03T05:55:16Z","timestamp":1585893316000},"page":"1438","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":12,"title":["A Fast and Validated High Throughput Bar Adsorptive Microextraction (HT-BA\u00b5E) Method for the Determination of Ketamine and Norketamine in Urine Samples"],"prefix":"10.3390","volume":"25","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-6921-1610","authenticated-orcid":false,"given":"Samir M.","family":"Ahmad","sequence":"first","affiliation":[{"name":"Centro de Qu\u00edmica Estrutural, Faculdade de Ci\u00eancias, Universidade de Lisboa, Campo Grande, 1749-016 Lisboa, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9079-9025","authenticated-orcid":false,"given":"Mariana N.","family":"Oliveira","sequence":"additional","affiliation":[{"name":"Centro de Qu\u00edmica Estrutural, Faculdade de Ci\u00eancias, Universidade de Lisboa, Campo Grande, 1749-016 Lisboa, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9879-1565","authenticated-orcid":false,"given":"Nuno R.","family":"Neng","sequence":"additional","affiliation":[{"name":"Centro de Qu\u00edmica Estrutural, Faculdade de Ci\u00eancias, Universidade de Lisboa, Campo Grande, 1749-016 Lisboa, Portugal"},{"name":"Departamento de Qu\u00edmica e Bioqu\u00edmica, Faculdade de Ci\u00eancias, Universidade de Lisboa, Campo Grande, 1749-016 Lisboa, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5785-6780","authenticated-orcid":false,"given":"J.M.F.","family":"Nogueira","sequence":"additional","affiliation":[{"name":"Centro de Qu\u00edmica Estrutural, Faculdade de Ci\u00eancias, Universidade de Lisboa, Campo Grande, 1749-016 Lisboa, Portugal"},{"name":"Departamento de Qu\u00edmica e Bioqu\u00edmica, Faculdade de Ci\u00eancias, Universidade de Lisboa, Campo Grande, 1749-016 Lisboa, Portugal"}]}],"member":"1968","published-online":{"date-parts":[[2020,3,22]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"2","DOI":"10.1080\/20961790.2017.1285219","article-title":"Metabolism and metabolomics of ketamine: A toxicological approach","volume":"2","year":"2017","journal-title":"Forensic Sci. Res."},{"key":"ref_2","unstructured":"Kuhar, M.J., and Liddle, H. (2012). Drugs of Abuse, Marshall Cavendish Reference. [1st ed.]."},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"47","DOI":"10.1016\/j.forsciint.2014.04.016","article-title":"Determination of ketamine, norketamine and dehydronorketamine in urine by hollow-fiber liquid-phase microextraction using an essential oil as supported liquid membrane","volume":"243","author":"Lanaro","year":"2014","journal-title":"Forensic Sci. Int."},{"key":"ref_4","unstructured":"World Drug Report 2019 (United Nations publication, Sales No. E.19.XI.8). Available online: https:\/\/wdr.unodc.org\/wdr2019\/."},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"27","DOI":"10.1093\/bja\/53.1.27","article-title":"Pharmacokinetics and analgesic effect of ketamine in man","volume":"53","author":"Clements","year":"1981","journal-title":"Br. J. Anaesth."},{"key":"ref_6","unstructured":"Karch, S. (2002). Pathology of Drug Abuse, CRC Press. [3rd ed.]."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"376","DOI":"10.1093\/jat\/29.5.376","article-title":"Urinary excretion rates of ketamine and norketamine following therapeutic ketamine administration: Method and detection window considerations","volume":"29","author":"Adamowicz","year":"2005","journal-title":"J. Anal. Toxicol."},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"583","DOI":"10.1093\/jat\/25.7.583","article-title":"Urine concentrations of ketamine and norketamine following illegal consumption","volume":"25","author":"Moore","year":"2001","journal-title":"J. Anal. Toxicol."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"7003","DOI":"10.1016\/j.chroma.2010.09.006","article-title":"PH-resistant titania hybrid organic-inorganic coating for stir bar sorptive extraction of drugs of abuse in urine samples followed by high performance liquid chromatography-ultraviolet visible detection","volume":"1217","author":"Lan","year":"2010","journal-title":"J. Chromatogr. A"},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"969","DOI":"10.1016\/j.talanta.2010.06.001","article-title":"Simultaneous quantification of amphetamines, caffeine and ketamine in urine by hollow fiber liquid phase microextraction combined with gas chromatography-flame ionization detector","volume":"82","author":"Xiong","year":"2010","journal-title":"Talanta"},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"443","DOI":"10.1016\/j.jchromb.2007.02.005","article-title":"GC-MS quantification of ketamine, norketamine, and dehydronorketamine in urine specimens and comparative study using ELISA as the preliminary test methodology","volume":"852","author":"Cheng","year":"2007","journal-title":"J. Chromatogr. B Anal. Technol. Biomed. Life Sci."},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"67","DOI":"10.1016\/j.jchromb.2015.09.032","article-title":"Determination of ketamine and its major metabolite, norketamine, in urine and plasma samples using microextraction by packed sorbent and gas chromatography-tandem mass spectrometry","volume":"1004","author":"Moreno","year":"2015","journal-title":"J. Chromatogr. B Anal. Technol. Biomed. Life Sci."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"87","DOI":"10.1016\/j.jpba.2017.02.035","article-title":"Quantitative chiral and achiral determination of ketamine and its metabolites by LC\u2013MS\/MS in human serum, urine and fecal samples","volume":"139","author":"Hasan","year":"2017","journal-title":"J. Pharm. Biomed. Anal."},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"679","DOI":"10.1093\/jat\/bkx057","article-title":"Simultaneous quantitation of methamphetamine, ketamine, opiates and their metabolites in urine by SPE and LC-MS-MS","volume":"41","author":"Yang","year":"2017","journal-title":"J. Anal. Toxicol."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"230","DOI":"10.1016\/j.jchromb.2016.03.040","article-title":"Simultaneous analysis method for GHB, ketamine, norketamine, phenobarbital, thiopental, zolpidem, zopiclone and phenytoin in urine, using C18 poroshell column","volume":"1022","author":"Anilanmert","year":"2016","journal-title":"J. Chromatogr. B Anal. Technol. Biomed. Life Sci."},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"142","DOI":"10.1016\/j.forsciint.2006.10.015","article-title":"A validated SPME-GC-MS method for simultaneous quantification of club drugs in human urine","volume":"171","author":"Brown","year":"2007","journal-title":"Forensic Sci. Int."},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"195","DOI":"10.1016\/j.talanta.2019.02.004","article-title":"High throughput bar adsorptive microextraction: A novel cost-effective tool for monitoring benzodiazepines in large number of biological samples","volume":"199","author":"Ahmad","year":"2019","journal-title":"Talanta"},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"17","DOI":"10.1016\/j.chroma.2019.04.035","article-title":"Bar adsorptive microextraction coated with multi-walled carbon nanotube phases\u2014Application for trace analysis of pharmaceuticals in environmental waters","volume":"1600","author":"Abujaber","year":"2019","journal-title":"J. Chromatogr. A"},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"126","DOI":"10.1016\/j.jpba.2018.02.001","article-title":"New-generation bar adsorptive microextraction (BA\u03bcE) devices for a better eco-user-friendly analytical approach\u2013Application for the determination of antidepressant pharmaceuticals in biological fluids","volume":"153","author":"Ide","year":"2018","journal-title":"J. Pharm. Biomed. Anal."},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"484","DOI":"10.1080\/03067319.2017.1324024","article-title":"Application of bar adsorptive microextraction to determine trace organic micro-pollutants in environmental water matrices","volume":"97","author":"Ahmad","year":"2017","journal-title":"Int. J. Environ. Anal. Chem."},{"key":"ref_21","doi-asserted-by":"crossref","unstructured":"Ahmad, S.M., Gomes, M.I., Ide, A.H., Neng, N.R., and Nogueira, J.M.F. (2019). Monitoring traces of organochlorine pesticides in herbal matrices by bar adsorptive microextraction\u2013Application to black tea and tobacco. Int. J. Environ. Anal. Chem., 1\u201315.","DOI":"10.1080\/03067319.2019.1682140"}],"container-title":["Molecules"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1420-3049\/25\/6\/1438\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,11]],"date-time":"2025-10-11T09:10:37Z","timestamp":1760173837000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1420-3049\/25\/6\/1438"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2020,3,22]]},"references-count":21,"journal-issue":{"issue":"6","published-online":{"date-parts":[[2020,3]]}},"alternative-id":["molecules25061438"],"URL":"https:\/\/doi.org\/10.3390\/molecules25061438","relation":{},"ISSN":["1420-3049"],"issn-type":[{"value":"1420-3049","type":"electronic"}],"subject":[],"published":{"date-parts":[[2020,3,22]]}}}