{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,3,25]],"date-time":"2026-03-25T19:00:23Z","timestamp":1774465223389,"version":"3.50.1"},"reference-count":39,"publisher":"MDPI AG","issue":"1","license":[{"start":{"date-parts":[[2021,1,13]],"date-time":"2021-01-13T00:00:00Z","timestamp":1610496000000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"name":"Fundaci\u00f3n S\u00e9neca, Spain","award":["19888\/GERM\/15"],"award-info":[{"award-number":["19888\/GERM\/15"]}]},{"name":"Ministry of Science","award":["PGC2018-098363-B-100"],"award-info":[{"award-number":["PGC2018-098363-B-100"]}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Toxins"],"abstract":"<jats:p>The use of dispersive liquid\u2013liquid microextraction (DLLME) is proposed for the preconcentration of thirteen lipophilic marine toxins in seawater samples. For this purpose, 0.5 mL of methanol and 440 \u00b5L of chloroform were injected into 12 mL of sample. The enriched organic phase, once evaporated and reconstituted in methanol, was analyzed by reversed-phase liquid chromatography with triple-quadrupole tandem mass spectrometry. A central composite design multivariate method was used to optimize the interrelated parameters affecting DLLME efficiency. The absence of any matrix effect in the samples allowed them to be quantified against aqueous standards. The optimized procedure was validated by recovery studies, which provided values in the 82\u2013123% range. The detection limits varied between 0.2 and 5.7 ng L\u22121, depending on the analyte, and the intraday precision values were in the 0.1\u20137.5% range in terms of relative standard deviation. Ten water samples taken from different points of the Mar Menor lagoon were analyzed and were found to be free of the studied toxins.<\/jats:p>","DOI":"10.3390\/toxins13010057","type":"journal-article","created":{"date-parts":[[2021,1,13]],"date-time":"2021-01-13T21:50:54Z","timestamp":1610574654000},"page":"57","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":10,"title":["Monitoring Lipophilic Toxins in Seawater Using Dispersive Liquid\u2014Liquid Microextraction and Liquid Chromatography with Triple Quadrupole Mass Spectrometry"],"prefix":"10.3390","volume":"13","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-7480-1001","authenticated-orcid":false,"given":"Ainhoa","family":"Oller-Ruiz","sequence":"first","affiliation":[{"name":"Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence \u201cCampus Mare Nostrum\u201d, University of Murcia, E-30100 Murcia, Spain"},{"name":"Department of Chemical and Environmental Engineering, Regional Campus of International Excellence \u201cCampus Mare Nostrum\u201d, Polytechnic University of Cartagena, E-30203 Cartagena, Spain"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Natalia","family":"Campillo","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence \u201cCampus Mare Nostrum\u201d, University of Murcia, E-30100 Murcia, Spain"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1795-3476","authenticated-orcid":false,"given":"Manuel","family":"Hern\u00e1ndez-C\u00f3rdoba","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence \u201cCampus Mare Nostrum\u201d, University of Murcia, E-30100 Murcia, Spain"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Javier","family":"Gilabert","sequence":"additional","affiliation":[{"name":"Department of Chemical and Environmental Engineering, Regional Campus of International Excellence \u201cCampus Mare Nostrum\u201d, Polytechnic University of Cartagena, E-30203 Cartagena, Spain"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5219-3711","authenticated-orcid":false,"given":"Pilar","family":"Vi\u00f1as","sequence":"additional","affiliation":[{"name":"Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence \u201cCampus Mare Nostrum\u201d, University of Murcia, E-30100 Murcia, Spain"}],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"1968","published-online":{"date-parts":[[2021,1,13]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"1653","DOI":"10.1007\/s00216-010-3779-4","article-title":"Advances in the detection of phycotoxins and cyanotoxins","volume":"397","author":"Humbert","year":"2010","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"30","DOI":"10.1016\/j.hal.2017.03.005","article-title":"High resolution mass spectrometry-based screening reveals lipophilic toxins in multiple trophic levels from the North Sea","volume":"64","author":"Orellana","year":"2017","journal-title":"Harmful Algae"},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"112","DOI":"10.1016\/j.hal.2016.02.008","article-title":"Distribution, occurrence and biotoxin composition of the main shellfish toxin producing microalgae within European waters: A comparison of methods of analysis","volume":"55","author":"McNamee","year":"2016","journal-title":"Harmful Algae"},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"189","DOI":"10.3390\/toxins11040189","article-title":"Dinophysis species and diarrhetic shellfish toxins: 20 years of monitoring program in Andalusia, South of spain","volume":"11","author":"Fuentes","year":"2019","journal-title":"Toxins"},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"1954","DOI":"10.3390\/w11091954","article-title":"Pseudo-nitzschia blooms in a coastal upwelling system: Remote sensing detection, toxicity and environmental variables","volume":"11","author":"Palenzuela","year":"2019","journal-title":"Water"},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"14266","DOI":"10.1007\/s11356-019-04660-x","article-title":"Long-term study of seasonal changes in phytoplankton community structure in the western Mediterranean (Valencian Community)","volume":"26","author":"Paches","year":"2019","journal-title":"Environ. Sci. Pollut. Res."},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"901","DOI":"10.1016\/j.scitotenv.2019.01.375","article-title":"Hydrogeological modelling for the watershed management of the Mar Menor coastal lagoon (Spain)","volume":"663","author":"Alcolea","year":"2019","journal-title":"Sci. Total Environ."},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"600","DOI":"10.3390\/jmse8080600","article-title":"Phytoplankton distribution in Mar Menor coastal lagoon (SE Spain) during 2017","volume":"8","author":"Soria","year":"2020","journal-title":"J. Mar. Sci. Eng."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"46","DOI":"10.3390\/md16020046","article-title":"Mixtures of lipophilic phycotoxins: exposure data and toxicological assessment","volume":"16","author":"Alarcan","year":"2018","journal-title":"Mar. Drugs"},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"1715","DOI":"10.1007\/s00216-010-3699-3","article-title":"A strategy to study genotoxicity: Application to aquatic toxins, limits and solutions","volume":"397","author":"Fessard","year":"2010","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_11","unstructured":"European Commission (2019). Regulation 2019\/627 of 15 March 2019 laying down uniform practical arrangements for the performance of official controls on products of animal origin intended for human consumption. Off. J. Eur. Union L, 131, 51\u2013100."},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"239","DOI":"10.1080\/026520399284000","article-title":"Use of immunoaffinity columns for clean-up of diarrhetic toxins (okadaic acid and dinophysistoxins) extracts from shellfish prior to their analysis by HPLC\/fluorimetry","volume":"16","author":"Puech","year":"1999","journal-title":"Food Addit. Contam."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"555","DOI":"10.1093\/jaoac\/78.2.555","article-title":"Analysis of diarrhetic shellfish poisoning toxins in shellfish tissue by liquid chromatography with fluorometric and mass spectrometric detection","volume":"78","author":"Quilliam","year":"1995","journal-title":"J. AOAC Int."},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"533","DOI":"10.1016\/j.foodchem.2011.04.054","article-title":"Automated on-line solid-phase extraction coupled to liquid chromatography-tandem mass spectrometry for determination of lipophilic marine toxins in shellfish","volume":"129","author":"Regueiro","year":"2011","journal-title":"Food Chem."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"770","DOI":"10.1016\/j.talanta.2013.07.042","article-title":"Graphene based pipette tip solid phase extraction of marine toxins in shellfish muscle followed by UPLC-MS\/MS analysis","volume":"116","author":"Shen","year":"2013","journal-title":"Talanta"},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"4529","DOI":"10.1016\/j.chroma.2009.03.062","article-title":"Sensitive method for the determination of lipophilic marine biotoxins in extracts of mussels and processed shellfish by high-performance liquid chromatography-tandem mass spectrometry based on enrichment by solid-phase extraction","volume":"1216","author":"These","year":"2009","journal-title":"J. Chromatogr. A"},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"427","DOI":"10.1016\/j.foodchem.2018.08.071","article-title":"Determination of lipophilic marine toxins in fresh and processed shellfish using modified QuEChERS and ultra-high-performance liquid chromatography\u2013tandem mass spectrometry","volume":"272","author":"Wang","year":"2019","journal-title":"Food Chem."},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"273","DOI":"10.1016\/j.chroma.2007.05.016","article-title":"Development of an ultra-performance liquid chromatography-mass spectrometry method for the detection of lipophilic marine toxins","volume":"1157","author":"Fux","year":"2007","journal-title":"J. Chromatogr. A"},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"4281","DOI":"10.3390\/md13074281","article-title":"Distribution of marine lipophilic toxins in shellfish products collected from the chinese market","volume":"13","author":"Wu","year":"2015","journal-title":"Mar. Drugs"},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"353","DOI":"10.1016\/S0021-9673(02)00545-9","article-title":"Comparison of solid-phase extraction methods for the determination of azaspiracids in shellfish by liquid chromatography-electrospray mass spectrometry","volume":"963","author":"Moroney","year":"2002","journal-title":"J. Chromatogr. A"},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"954","DOI":"10.1016\/j.marpolbul.2015.10.038","article-title":"Determination of typical lipophilic marine toxins in marine sediments from three coastal bays of China using liquid chromatography-tandem mass spectrometry after accelerated solvent extraction","volume":"101","author":"Wang","year":"2015","journal-title":"Mar. Pollut. Bull."},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"32","DOI":"10.1016\/j.chemosphere.2016.10.052","article-title":"Screening of lipophilic marine toxins in marine aquaculture environment using liquid chromatography-mass spectrometry","volume":"168","author":"Chen","year":"2017","journal-title":"Chemosphere"},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"526","DOI":"10.1016\/j.microc.2018.02.005","article-title":"Polymeric ion exchange material based dispersive micro solid-phase extraction of lipophilic marine toxins in seawater followed by the Q Exactive mass spectrometer analysis using a scheduled high resolution parallel reaction monitoring","volume":"138","author":"Zhang","year":"2018","journal-title":"Microchem. J."},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"380","DOI":"10.1016\/j.chemosphere.2017.05.073","article-title":"Lipophilic marine toxins discovered in the Bohai Sea using high performance liquid chromatography coupled with tandem mass spectrometry","volume":"183","author":"Liu","year":"2017","journal-title":"Chemosphere"},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"543","DOI":"10.1093\/jaoac\/78.2.543","article-title":"Rapid extraction and cleanup for liquid chromatography determination of domoic acid in unsalted seafood","volume":"78","author":"Quilliam","year":"1995","journal-title":"J. AOAC Int."},{"key":"ref_26","doi-asserted-by":"crossref","first-page":"931","DOI":"10.1016\/j.scitotenv.2017.08.304","article-title":"Occurrence and distribution of marine natural organic pollutants: Lipophilic marine algal toxins in the Yellow Sea and the Bohai Sea, China","volume":"612","author":"Chen","year":"2018","journal-title":"Sci. Total Environ."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"560","DOI":"10.1016\/j.chemosphere.2014.05.006","article-title":"Detection, occurrence and monthly variations of typical lipophilic marine toxins associated with diarrhetic shellfish poisoning in the coastal seawater of Qingdao City, China","volume":"111","author":"Li","year":"2014","journal-title":"Chemosphere"},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"5451","DOI":"10.1007\/s00216-017-0536-y","article-title":"Analysis of lipophilic marine biotoxins by liquid chromatography coupled with high-resolution mass spectrometry in seawater from the Catalan Coast","volume":"409","year":"2017","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"16","DOI":"10.1016\/j.toxicon.2016.02.011","article-title":"Algal toxin profiles in Nigerian coastal waters (Gulf of Guinea) using passive sampling and liquid chromatography coupled to mass spectrometry","volume":"114","author":"Zendong","year":"2016","journal-title":"Toxicon"},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"104","DOI":"10.1016\/j.foodchem.2019.05.031","article-title":"Reversed-phase\/weak anion exchange magnetic mesoporous microspheres for removal of matrix effects in lipophilic marine biotoxins analysis by ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry","volume":"294","author":"Xu","year":"2019","journal-title":"Food Chem."},{"key":"ref_31","doi-asserted-by":"crossref","unstructured":"Gim\u00e9nez-Campillo, C., Pastor-Belda, M., Campillo, N., Arroyo-Manzanares, N., Hern\u00e1ndez-C\u00f3rdoba, M., and Vi\u00f1as, P. (2019). Determination of cyanotoxins and phycotoxins in seawater and algae-based food supplements using ionic liquids and liquid chromatography with time-of-flight mass spectrometry. Toxins, 11.","DOI":"10.3390\/toxins11100610"},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"1213","DOI":"10.1007\/s00216-009-2790-0","article-title":"Solid phase extraction for removal of matrix effects in lipophilic marine toxin analysis by liquid chromatography-tandem mass spectrometry","volume":"394","author":"Gerssen","year":"2009","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_33","doi-asserted-by":"crossref","first-page":"622","DOI":"10.1016\/j.talanta.2018.07.050","article-title":"A single run UPLC-MS\/MS method for detection of all EU-regulated marine toxins","volume":"189","author":"Alfonso","year":"2018","journal-title":"Talanta"},{"key":"ref_34","doi-asserted-by":"crossref","first-page":"16","DOI":"10.1016\/j.chroma.2013.12.071","article-title":"Determination of lipophilic marine toxins in mussels. Quantification and confirmation criteria using high resolution mass spectrometry","volume":"1328","author":"Palacios","year":"2014","journal-title":"J. Chromatogr. A"},{"key":"ref_35","doi-asserted-by":"crossref","first-page":"3116","DOI":"10.1007\/s11356-014-3595-z","article-title":"Lipophilic shellfish toxins in Dinophysis caudata picked cells and in shellfish from the East China Sea","volume":"22","author":"Li","year":"2015","journal-title":"Environ. Sci. Pollut. Res."},{"key":"ref_36","doi-asserted-by":"crossref","first-page":"6345","DOI":"10.1007\/s00216-015-8637-y","article-title":"Quantification and profiling of lipophilic marine toxins in microalgae by UHPLC coupled to high-resolution orbitrap mass spectrometry","volume":"407","author":"Orellana","year":"2015","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_37","doi-asserted-by":"crossref","first-page":"797","DOI":"10.1007\/s00216-008-2221-7","article-title":"LC-MS-MS aboard ship: Tandem mass spectrometry in the search for phycotoxins and novel toxigenic plankton from the North Sea","volume":"392","author":"Krock","year":"2008","journal-title":"Anal. Bioanal. Chem."},{"key":"ref_38","doi-asserted-by":"crossref","first-page":"316","DOI":"10.5740\/jaoacint.SGEMcCarron","article-title":"Liquid chromatography\/mass spectrometry of domoic acid and lipophilic shellfish toxins with selected reaction monitoring and optional confirmation by library searching of product ion spectra","volume":"97","author":"McCarron","year":"2014","journal-title":"J. AOAC Int."},{"key":"ref_39","doi-asserted-by":"crossref","unstructured":"Josi\u0107, D., Re\u0161etar, D., Per\u0161uri\u0107, \u017d., Martinovi\u0107, T., and Kraljevic Paveli\u0107, S. (2017). Detection of microbial toxins by -omics methods: A growing role of proteomics. Proteomics for Microbial Toxin Identification, Elsevier.","DOI":"10.1016\/B978-0-12-804007-2.00029-1"}],"container-title":["Toxins"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/2072-6651\/13\/1\/57\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,11]],"date-time":"2025-10-11T05:10:49Z","timestamp":1760159449000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/2072-6651\/13\/1\/57"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2021,1,13]]},"references-count":39,"journal-issue":{"issue":"1","published-online":{"date-parts":[[2021,1]]}},"alternative-id":["toxins13010057"],"URL":"https:\/\/doi.org\/10.3390\/toxins13010057","relation":{},"ISSN":["2072-6651"],"issn-type":[{"value":"2072-6651","type":"electronic"}],"subject":[],"published":{"date-parts":[[2021,1,13]]}}}