{"id":377,"date":"2019-12-10T16:29:35","date_gmt":"2019-12-10T15:29:35","guid":{"rendered":"https:\/\/wpd.ugr.es\/~fqm302\/blog\/?p=377"},"modified":"2019-12-10T16:29:35","modified_gmt":"2019-12-10T15:29:35","slug":"monitoring-of-cyanotoxins-in-water-from-hypersaline-microalgae-colonies-by-ultra-high-performance-liquid-chromatography-with-diode-array-and-tandem-mass-spectrometry-detection-following-salting-out-li","status":"publish","type":"post","link":"https:\/\/wpd.ugr.es\/~fqm302\/blog\/?p=377","title":{"rendered":"Monitoring of cyanotoxins in water from hypersaline microalgae colonies by ultra high performance liquid chromatography with diode array and tandem mass spectrometry detection following salting-out liquid-liquid extraction."},"content":{"rendered":"<p>In this study two different analytical approaches have been developed to determine the presence of several cyanotoxins in saline water samples from a continental salt marsh. A salting-out assisted liquid-liquid extraction (SALLE) has been used in combination with ultra-high performance liquid chromatography-tandem mass spectrometry and UV-diode array detection (UHPLC-MS\/MS and UHPLC-DAD). The target analytes are eight microcystins named MC-RR, MC-YR, MC-LR, MC-WR, MC-LA, MC-LY, MC-LW, MC-LF and nodularin (NOD), covering a wide range of polarities. The separation was achieved using a Zorbax Eclipse Plus RRHD C18 column (50\u202f\u00d7\u202f2.1\u202fmm, 1.8\u202f\u03bcm) in less than 7.5 and 5.5\u202fmin for UV and MS\/MS detection, respectively. The mobile phase used consisted of water (solvent A) and acetonitrile (MeCN) (solvent B), both containing 0.01% of formic acid for DAD and 0.4% of formic acid for MS\/MS detection, at a flow rate of 0.4\u202fmL min<sup>\u22121<\/sup>. The temperature of the column was set at 25\u202f\u00b0C and 20\u202f\u03bcL of sample were injected. The main parameters affecting the SALLE procedure were studied and the following optimum values were obtained: neutral pH, 2\u202fmL of acetonitrile as extraction solvent and 1.2\u202fg of ammonium sulfate as salting-out agent for 4\u202fmL of water sample. The validation protocols for both methods were accomplished with real water samples obtaining LODs ranging from 1.0 to 3.4\u202f\u03bcg L<sup>\u22121<\/sup>\u00a0and 0.02 to 0.11\u202f\u03bcg L<sup>\u22121<\/sup>\u00a0for DAD and MS\/MS respectively. Although the SALLE-UHPLC-DAD methodology is easier and cheaper than UHPLC-MS\/MS significantly better detection limits were achieved with tandem mass spectrometry as well as allowing for unambiguous identification. Extraction recoveries were higher than 77.0% (except for MC-RR and NOD which were 53.2% and 54.3, respectively) with satisfactory inter-day and intra-day precisions (RSD below 13.3%).<\/p>\n","protected":false},"excerpt":{"rendered":"<p>In this study two different analytical approaches have been developed to determine the presence of several cyanotoxins in saline water samples from a continental salt marsh. A salting-out assisted liquid-liquid extraction (SALLE) has been used in combination with ultra-high performance &hellip; <a href=\"https:\/\/wpd.ugr.es\/~fqm302\/blog\/?p=377\">Continue reading <span class=\"meta-nav\">&rarr;<\/span><\/a><\/p>\n","protected":false},"author":2,"featured_media":0,"comment_status":"closed","ping_status":"closed","sticky":false,"template":"","format":"standard","meta":{"footnotes":""},"categories":[155,26,154,87,57,58,62],"tags":[101,104,107,108],"class_list":["post-377","post","type-post","status-publish","format-standard","hentry","category-cyanotoxins","category-mass-spectrometry","category-rti2018-097043-b-i00","category-salle","category-uhplc","category-uv-vis","category-water","tag-ms","tag-salle","tag-uhplc","tag-uv-vis-2"],"_links":{"self":[{"href":"https:\/\/wpd.ugr.es\/~fqm302\/blog\/index.php?rest_route=\/wp\/v2\/posts\/377","targetHints":{"allow":["GET"]}}],"collection":[{"href":"https:\/\/wpd.ugr.es\/~fqm302\/blog\/index.php?rest_route=\/wp\/v2\/posts"}],"about":[{"href":"https:\/\/wpd.ugr.es\/~fqm302\/blog\/index.php?rest_route=\/wp\/v2\/types\/post"}],"author":[{"embeddable":true,"href":"https:\/\/wpd.ugr.es\/~fqm302\/blog\/index.php?rest_route=\/wp\/v2\/users\/2"}],"replies":[{"embeddable":true,"href":"https:\/\/wpd.ugr.es\/~fqm302\/blog\/index.php?rest_route=%2Fwp%2Fv2%2Fcomments&post=377"}],"version-history":[{"count":1,"href":"https:\/\/wpd.ugr.es\/~fqm302\/blog\/index.php?rest_route=\/wp\/v2\/posts\/377\/revisions"}],"predecessor-version":[{"id":378,"href":"https:\/\/wpd.ugr.es\/~fqm302\/blog\/index.php?rest_route=\/wp\/v2\/posts\/377\/revisions\/378"}],"wp:attachment":[{"href":"https:\/\/wpd.ugr.es\/~fqm302\/blog\/index.php?rest_route=%2Fwp%2Fv2%2Fmedia&parent=377"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/wpd.ugr.es\/~fqm302\/blog\/index.php?rest_route=%2Fwp%2Fv2%2Fcategories&post=377"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/wpd.ugr.es\/~fqm302\/blog\/index.php?rest_route=%2Fwp%2Fv2%2Ftags&post=377"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}