Optimization of solid-phase extraction and liquid chromatography–tandem mass spectrometry for the determination of domoic acid in seawater, phytoplankton, and mammalian fluids and tissues
[Display omitted] ► Reversed-phase solid-phase extraction (SPE) was applied for domoic acid extraction and clean-up for LC–MS quantitation. ► An SPE cartridge instead of disk format was used to avoid DA loss during seawater sample loading. ► 20-Fold DA pre-concentration in seawater with/without phyt...
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| creator | Wang, Zhihong Maucher-Fuquay, Jennifer Fire, Spencer E. Mikulski, Christina M. Haynes, Bennie Doucette, Gregory J. Ramsdell, John S. |
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► Reversed-phase solid-phase extraction (SPE) was applied for domoic acid extraction and clean-up for LC–MS quantitation. ► An SPE cartridge instead of disk format was used to avoid DA loss during seawater sample loading. ► 20-Fold DA pre-concentration in seawater with/without phytoplankton was achieved after SPE method improvement. ► The SPE method for seawater was modified and extended to mammalian fluids and tissues for LC–MS analysis.
We previously reported a solid-phase extraction (SPE) method for determination of the neurotoxin domoic acid (DA) in both seawater and phytoplankton by liquid chromatography–tandem mass spectrometry (LC–MS/MS) with the purpose of sample desalting without DA pre-concentration. In the present study, we optimized the SPE procedure with seawater and phytoplankton samples directly acidified with aqueous formic acid without addition of organic solvents, which allowed sample desalting and also 20-fold pre-concentration of DA in seawater and phytoplankton samples. In order to reduce MS contamination, a diverter valve was installed between LC and MS to send the LC eluant to waste, except for the 6-min elution window bracketing the DA retention time, which was sent to the MS. Reduction of the MS turbo gas temperature also helped to maintain the long-term stability of MS signal. Recoveries exceeded 90% for the DA-negative seawater and the DA-positive cultured phytoplankton samples spiked with DA. The SPE method for DA extraction and sample clean-up in seawater was extended to mammalian fluids and tissues with modification in order to accommodate the fluid samples with limited available volumes and the tissue extracts in aqueous methanol. Recoveries of DA from DA-exposed laboratory mammalian samples (amniotic fluid, cerebrospinal fluid, plasma, placenta, and brain) were above 85%. Recoveries of DA from samples (urine, feces, intestinal contents, and gastric contents) collected from field stranded marine mammals showed large variations and were affected by the sample status. The optimized SPE–LC–MS method allows determination of DA at trace levels (low pg
mL
−1) in seawater with/without the presence of phytoplankton. The application of SPE clean-up to mammalian fluids and tissue extracts greatly reduced the LC column degradation and MS contamination, which allowed routine screening of marine mammalian samples for confirmation of DA exposure and determination of fluid and tissue DA concentrations in experimental labor |
| doi_str_mv | 10.1016/j.aca.2011.12.013 |
| format | Article |
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► Reversed-phase solid-phase extraction (SPE) was applied for domoic acid extraction and clean-up for LC–MS quantitation. ► An SPE cartridge instead of disk format was used to avoid DA loss during seawater sample loading. ► 20-Fold DA pre-concentration in seawater with/without phytoplankton was achieved after SPE method improvement. ► The SPE method for seawater was modified and extended to mammalian fluids and tissues for LC–MS analysis.
We previously reported a solid-phase extraction (SPE) method for determination of the neurotoxin domoic acid (DA) in both seawater and phytoplankton by liquid chromatography–tandem mass spectrometry (LC–MS/MS) with the purpose of sample desalting without DA pre-concentration. In the present study, we optimized the SPE procedure with seawater and phytoplankton samples directly acidified with aqueous formic acid without addition of organic solvents, which allowed sample desalting and also 20-fold pre-concentration of DA in seawater and phytoplankton samples. In order to reduce MS contamination, a diverter valve was installed between LC and MS to send the LC eluant to waste, except for the 6-min elution window bracketing the DA retention time, which was sent to the MS. Reduction of the MS turbo gas temperature also helped to maintain the long-term stability of MS signal. Recoveries exceeded 90% for the DA-negative seawater and the DA-positive cultured phytoplankton samples spiked with DA. The SPE method for DA extraction and sample clean-up in seawater was extended to mammalian fluids and tissues with modification in order to accommodate the fluid samples with limited available volumes and the tissue extracts in aqueous methanol. Recoveries of DA from DA-exposed laboratory mammalian samples (amniotic fluid, cerebrospinal fluid, plasma, placenta, and brain) were above 85%. Recoveries of DA from samples (urine, feces, intestinal contents, and gastric contents) collected from field stranded marine mammals showed large variations and were affected by the sample status. The optimized SPE–LC–MS method allows determination of DA at trace levels (low pg
mL
−1) in seawater with/without the presence of phytoplankton. The application of SPE clean-up to mammalian fluids and tissue extracts greatly reduced the LC column degradation and MS contamination, which allowed routine screening of marine mammalian samples for confirmation of DA exposure and determination of fluid and tissue DA concentrations in experimental laboratory animals.</description><identifier>ISSN: 0003-2670</identifier><identifier>EISSN: 1873-4324</identifier><identifier>DOI: 10.1016/j.aca.2011.12.013</identifier><identifier>PMID: 22244169</identifier><identifier>CODEN: ACACAM</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Amniotic Fluid - chemistry ; Analysis methods ; Analytical chemistry ; Animals ; Applied sciences ; Body Fluids - chemistry ; Chemistry ; Chromatographic methods and physical methods associated with chromatography ; Chromatography, High Pressure Liquid - methods ; Cleaning ; Dolphins - urine ; Domoic acid ; Exact sciences and technology ; Extraction ; Feces - chemistry ; Female ; Fluid dynamics ; Fluid flow ; Fluids ; Kainic Acid - analogs & derivatives ; Kainic Acid - analysis ; Liquid chromatography–mass spectrometry ; Mammalian fluids and tissues ; Marine Toxins - analysis ; Other chromatographic methods ; Phytoplankton ; Phytoplankton - chemistry ; Pollution ; Rats ; Rats, Sprague-Dawley ; Recovery ; Sea Lions - urine ; Sea water ; Seawater ; Seawater - chemistry ; Sensitivity and Specificity ; Solid Phase Extraction - methods ; Solid-phase extraction ; Spectrometric and optical methods ; Tandem Mass Spectrometry - methods ; Wastes ; Whales - urine</subject><ispartof>Analytica chimica acta, 2012-02, Vol.715, p.71-79</ispartof><rights>2011 Elsevier B.V.</rights><rights>2015 INIST-CNRS</rights><rights>Copyright © 2011 Elsevier B.V. All rights reserved.</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c447t-64f39dff0eba8324ac86f04c4a179bbf993d409fed3d067842c3fa27f5de50f73</citedby><cites>FETCH-LOGICAL-c447t-64f39dff0eba8324ac86f04c4a179bbf993d409fed3d067842c3fa27f5de50f73</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://www.sciencedirect.com/science/article/pii/S0003267011016783$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,776,780,3537,27901,27902,65306</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=25642456$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/22244169$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Wang, Zhihong</creatorcontrib><creatorcontrib>Maucher-Fuquay, Jennifer</creatorcontrib><creatorcontrib>Fire, Spencer E.</creatorcontrib><creatorcontrib>Mikulski, Christina M.</creatorcontrib><creatorcontrib>Haynes, Bennie</creatorcontrib><creatorcontrib>Doucette, Gregory J.</creatorcontrib><creatorcontrib>Ramsdell, John S.</creatorcontrib><title>Optimization of solid-phase extraction and liquid chromatography–tandem mass spectrometry for the determination of domoic acid in seawater, phytoplankton, and mammalian fluids and tissues</title><title>Analytica chimica acta</title><addtitle>Anal Chim Acta</addtitle><description>[Display omitted]
► Reversed-phase solid-phase extraction (SPE) was applied for domoic acid extraction and clean-up for LC–MS quantitation. ► An SPE cartridge instead of disk format was used to avoid DA loss during seawater sample loading. ► 20-Fold DA pre-concentration in seawater with/without phytoplankton was achieved after SPE method improvement. ► The SPE method for seawater was modified and extended to mammalian fluids and tissues for LC–MS analysis.
We previously reported a solid-phase extraction (SPE) method for determination of the neurotoxin domoic acid (DA) in both seawater and phytoplankton by liquid chromatography–tandem mass spectrometry (LC–MS/MS) with the purpose of sample desalting without DA pre-concentration. In the present study, we optimized the SPE procedure with seawater and phytoplankton samples directly acidified with aqueous formic acid without addition of organic solvents, which allowed sample desalting and also 20-fold pre-concentration of DA in seawater and phytoplankton samples. In order to reduce MS contamination, a diverter valve was installed between LC and MS to send the LC eluant to waste, except for the 6-min elution window bracketing the DA retention time, which was sent to the MS. Reduction of the MS turbo gas temperature also helped to maintain the long-term stability of MS signal. Recoveries exceeded 90% for the DA-negative seawater and the DA-positive cultured phytoplankton samples spiked with DA. The SPE method for DA extraction and sample clean-up in seawater was extended to mammalian fluids and tissues with modification in order to accommodate the fluid samples with limited available volumes and the tissue extracts in aqueous methanol. Recoveries of DA from DA-exposed laboratory mammalian samples (amniotic fluid, cerebrospinal fluid, plasma, placenta, and brain) were above 85%. Recoveries of DA from samples (urine, feces, intestinal contents, and gastric contents) collected from field stranded marine mammals showed large variations and were affected by the sample status. The optimized SPE–LC–MS method allows determination of DA at trace levels (low pg
mL
−1) in seawater with/without the presence of phytoplankton. The application of SPE clean-up to mammalian fluids and tissue extracts greatly reduced the LC column degradation and MS contamination, which allowed routine screening of marine mammalian samples for confirmation of DA exposure and determination of fluid and tissue DA concentrations in experimental laboratory animals.</description><subject>Amniotic Fluid - chemistry</subject><subject>Analysis methods</subject><subject>Analytical chemistry</subject><subject>Animals</subject><subject>Applied sciences</subject><subject>Body Fluids - chemistry</subject><subject>Chemistry</subject><subject>Chromatographic methods and physical methods associated with chromatography</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Cleaning</subject><subject>Dolphins - urine</subject><subject>Domoic acid</subject><subject>Exact sciences and technology</subject><subject>Extraction</subject><subject>Feces - chemistry</subject><subject>Female</subject><subject>Fluid dynamics</subject><subject>Fluid flow</subject><subject>Fluids</subject><subject>Kainic Acid - analogs & derivatives</subject><subject>Kainic Acid - analysis</subject><subject>Liquid chromatography–mass spectrometry</subject><subject>Mammalian fluids and tissues</subject><subject>Marine Toxins - analysis</subject><subject>Other chromatographic methods</subject><subject>Phytoplankton</subject><subject>Phytoplankton - chemistry</subject><subject>Pollution</subject><subject>Rats</subject><subject>Rats, Sprague-Dawley</subject><subject>Recovery</subject><subject>Sea Lions - urine</subject><subject>Sea water</subject><subject>Seawater</subject><subject>Seawater - chemistry</subject><subject>Sensitivity and Specificity</subject><subject>Solid Phase Extraction - methods</subject><subject>Solid-phase extraction</subject><subject>Spectrometric and optical methods</subject><subject>Tandem Mass Spectrometry - methods</subject><subject>Wastes</subject><subject>Whales - urine</subject><issn>0003-2670</issn><issn>1873-4324</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2012</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNp9kU1uFDEQhS0EIkPgAGyQNwgW6cZ2u7unlRWK-JMiZQNrq8YuMx7a7Y7tAYYVd-A8XIaT4MwMYZeVVa6v3ivVI-QpZzVnvHu1qUFDLRjnNRc14809suDLvqlkI-R9smCMNZXoenZCHqW0KaXgTD4kJ0IIKXk3LMjvqzk7735AdmGiwdIURmeqeQ0JKX7PEfS-A5Oho7veOkP1OgYPOXyOMK93f37-yqWJnnpIiaYZdS59zHFHbYg0r5EazBi9m25NTPDBaQq6yLmJJoRvUJAzWgRzmEeYvuQwne1dPXgPo4OJ2rHYp_1ndiltMT0mDyyMCZ8c31Py6e2bjxfvq8urdx8uXl9WWso-V520zWCsZbiCZTkN6GVnmdQSeD-sVnYYGiPZYNE0hnX9UgrdWBC9bQ22zPbNKXlx0J1juC6-WXmXNI5lUQzbpAbB-kEKLgv58k6Sdz2XS9GyoaD8gOoYUopo1Rydh7hTnKmbfNVGlXzVTb6KC1XyLTPPjvLblUdzO_Ev0AI8PwKQNIw2wqRd-s-1nRSy7Qp3fuCwnO2rw6iSdjhpNC6WBJUJ7o41_gL9WckR</recordid><startdate>20120217</startdate><enddate>20120217</enddate><creator>Wang, Zhihong</creator><creator>Maucher-Fuquay, Jennifer</creator><creator>Fire, Spencer E.</creator><creator>Mikulski, Christina M.</creator><creator>Haynes, Bennie</creator><creator>Doucette, Gregory J.</creator><creator>Ramsdell, John S.</creator><general>Elsevier B.V</general><general>Elsevier</general><scope>IQODW</scope><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7U5</scope><scope>8FD</scope><scope>L7M</scope><scope>7ST</scope><scope>7TV</scope><scope>C1K</scope><scope>F1W</scope><scope>H97</scope><scope>L.G</scope><scope>M7N</scope><scope>SOI</scope></search><sort><creationdate>20120217</creationdate><title>Optimization of solid-phase extraction and liquid chromatography–tandem mass spectrometry for the determination of domoic acid in seawater, phytoplankton, and mammalian fluids and tissues</title><author>Wang, Zhihong ; Maucher-Fuquay, Jennifer ; Fire, Spencer E. ; Mikulski, Christina M. ; Haynes, Bennie ; Doucette, Gregory J. ; Ramsdell, John S.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c447t-64f39dff0eba8324ac86f04c4a179bbf993d409fed3d067842c3fa27f5de50f73</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2012</creationdate><topic>Amniotic Fluid - chemistry</topic><topic>Analysis methods</topic><topic>Analytical chemistry</topic><topic>Animals</topic><topic>Applied sciences</topic><topic>Body Fluids - chemistry</topic><topic>Chemistry</topic><topic>Chromatographic methods and physical methods associated with chromatography</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Cleaning</topic><topic>Dolphins - urine</topic><topic>Domoic acid</topic><topic>Exact sciences and technology</topic><topic>Extraction</topic><topic>Feces - chemistry</topic><topic>Female</topic><topic>Fluid dynamics</topic><topic>Fluid flow</topic><topic>Fluids</topic><topic>Kainic Acid - analogs & derivatives</topic><topic>Kainic Acid - analysis</topic><topic>Liquid chromatography–mass spectrometry</topic><topic>Mammalian fluids and tissues</topic><topic>Marine Toxins - analysis</topic><topic>Other chromatographic methods</topic><topic>Phytoplankton</topic><topic>Phytoplankton - chemistry</topic><topic>Pollution</topic><topic>Rats</topic><topic>Rats, Sprague-Dawley</topic><topic>Recovery</topic><topic>Sea Lions - urine</topic><topic>Sea water</topic><topic>Seawater</topic><topic>Seawater - chemistry</topic><topic>Sensitivity and Specificity</topic><topic>Solid Phase Extraction - methods</topic><topic>Solid-phase extraction</topic><topic>Spectrometric and optical methods</topic><topic>Tandem Mass Spectrometry - methods</topic><topic>Wastes</topic><topic>Whales - urine</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Wang, Zhihong</creatorcontrib><creatorcontrib>Maucher-Fuquay, Jennifer</creatorcontrib><creatorcontrib>Fire, Spencer E.</creatorcontrib><creatorcontrib>Mikulski, Christina M.</creatorcontrib><creatorcontrib>Haynes, Bennie</creatorcontrib><creatorcontrib>Doucette, Gregory J.</creatorcontrib><creatorcontrib>Ramsdell, John S.</creatorcontrib><collection>Pascal-Francis</collection><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>Technology Research Database</collection><collection>Advanced Technologies Database with Aerospace</collection><collection>Environment Abstracts</collection><collection>Pollution Abstracts</collection><collection>Environmental Sciences and Pollution Management</collection><collection>ASFA: Aquatic Sciences and Fisheries Abstracts</collection><collection>Aquatic Science & Fisheries Abstracts (ASFA) 3: Aquatic Pollution & Environmental Quality</collection><collection>Aquatic Science & Fisheries Abstracts (ASFA) Professional</collection><collection>Algology Mycology and Protozoology Abstracts (Microbiology C)</collection><collection>Environment Abstracts</collection><jtitle>Analytica chimica acta</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Wang, Zhihong</au><au>Maucher-Fuquay, Jennifer</au><au>Fire, Spencer E.</au><au>Mikulski, Christina M.</au><au>Haynes, Bennie</au><au>Doucette, Gregory J.</au><au>Ramsdell, John S.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Optimization of solid-phase extraction and liquid chromatography–tandem mass spectrometry for the determination of domoic acid in seawater, phytoplankton, and mammalian fluids and tissues</atitle><jtitle>Analytica chimica acta</jtitle><addtitle>Anal Chim Acta</addtitle><date>2012-02-17</date><risdate>2012</risdate><volume>715</volume><spage>71</spage><epage>79</epage><pages>71-79</pages><issn>0003-2670</issn><eissn>1873-4324</eissn><coden>ACACAM</coden><abstract>[Display omitted]
► Reversed-phase solid-phase extraction (SPE) was applied for domoic acid extraction and clean-up for LC–MS quantitation. ► An SPE cartridge instead of disk format was used to avoid DA loss during seawater sample loading. ► 20-Fold DA pre-concentration in seawater with/without phytoplankton was achieved after SPE method improvement. ► The SPE method for seawater was modified and extended to mammalian fluids and tissues for LC–MS analysis.
We previously reported a solid-phase extraction (SPE) method for determination of the neurotoxin domoic acid (DA) in both seawater and phytoplankton by liquid chromatography–tandem mass spectrometry (LC–MS/MS) with the purpose of sample desalting without DA pre-concentration. In the present study, we optimized the SPE procedure with seawater and phytoplankton samples directly acidified with aqueous formic acid without addition of organic solvents, which allowed sample desalting and also 20-fold pre-concentration of DA in seawater and phytoplankton samples. In order to reduce MS contamination, a diverter valve was installed between LC and MS to send the LC eluant to waste, except for the 6-min elution window bracketing the DA retention time, which was sent to the MS. Reduction of the MS turbo gas temperature also helped to maintain the long-term stability of MS signal. Recoveries exceeded 90% for the DA-negative seawater and the DA-positive cultured phytoplankton samples spiked with DA. The SPE method for DA extraction and sample clean-up in seawater was extended to mammalian fluids and tissues with modification in order to accommodate the fluid samples with limited available volumes and the tissue extracts in aqueous methanol. Recoveries of DA from DA-exposed laboratory mammalian samples (amniotic fluid, cerebrospinal fluid, plasma, placenta, and brain) were above 85%. Recoveries of DA from samples (urine, feces, intestinal contents, and gastric contents) collected from field stranded marine mammals showed large variations and were affected by the sample status. The optimized SPE–LC–MS method allows determination of DA at trace levels (low pg
mL
−1) in seawater with/without the presence of phytoplankton. The application of SPE clean-up to mammalian fluids and tissue extracts greatly reduced the LC column degradation and MS contamination, which allowed routine screening of marine mammalian samples for confirmation of DA exposure and determination of fluid and tissue DA concentrations in experimental laboratory animals.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>22244169</pmid><doi>10.1016/j.aca.2011.12.013</doi><tpages>9</tpages></addata></record> |
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| ispartof | Analytica chimica acta, 2012-02, Vol.715, p.71-79 |
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| source | MEDLINE; Elsevier ScienceDirect Journals |
| subjects | Amniotic Fluid - chemistry Analysis methods Analytical chemistry Animals Applied sciences Body Fluids - chemistry Chemistry Chromatographic methods and physical methods associated with chromatography Chromatography, High Pressure Liquid - methods Cleaning Dolphins - urine Domoic acid Exact sciences and technology Extraction Feces - chemistry Female Fluid dynamics Fluid flow Fluids Kainic Acid - analogs & derivatives Kainic Acid - analysis Liquid chromatography–mass spectrometry Mammalian fluids and tissues Marine Toxins - analysis Other chromatographic methods Phytoplankton Phytoplankton - chemistry Pollution Rats Rats, Sprague-Dawley Recovery Sea Lions - urine Sea water Seawater Seawater - chemistry Sensitivity and Specificity Solid Phase Extraction - methods Solid-phase extraction Spectrometric and optical methods Tandem Mass Spectrometry - methods Wastes Whales - urine |
| title | Optimization of solid-phase extraction and liquid chromatography–tandem mass spectrometry for the determination of domoic acid in seawater, phytoplankton, and mammalian fluids and tissues |
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