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Identification and Quantification of Loline-Type Alkaloids in Endophyte-Infected Grasses by LC-MS/MS
Lolines, fungal metabolites of the grass–endophyte association, were identified and quantified using newly developed LC-MS/MS methods in endophyte-infected grasses belonging to the Lolium and Festuca genera after extraction with three different solvents using two extraction methods. The shaking extr...
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Published in: | Journal of agricultural and food chemistry 2016-08, Vol.64 (31), p.6212-6218 |
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container_title | Journal of agricultural and food chemistry |
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creator | Adhikari, Khem B. Boelt, Birte Fomsgaard, Inge S. |
description | Lolines, fungal metabolites of the grass–endophyte association, were identified and quantified using newly developed LC-MS/MS methods in endophyte-infected grasses belonging to the Lolium and Festuca genera after extraction with three different solvents using two extraction methods. The shaking extraction method with isopropanol/water was superior to the other methods due to its high sensitivity, high accuracy (recovery within or close to the range of 80–120%), and high precision (coefficient of variation of |
doi_str_mv | 10.1021/acs.jafc.6b02616 |
format | article |
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The shaking extraction method with isopropanol/water was superior to the other methods due to its high sensitivity, high accuracy (recovery within or close to the range of 80–120%), and high precision (coefficient of variation of <10%). Seven loline alkaloids were identified and quantified using our newly established LC-MS/MS methods, and N-formylloline was the most abundant (5 mg/g dry matter), followed by N-acetylloline. These LC-MS/MS methods used the shortest sample handling time and the fewest sample preparation steps and proved to be good alternatives to existing GC and GC-MS analytical methods without compromising analytical efficiency. In conclusion, we developed for the first time a highly sensitive quantitative LC-MS/MS analytical method for the accurate and reproducible quantification and a LightSight-assisted LC-QTRAP/MS qualitative method for the tentative identification of loline-type alkaloids in endophyte-infected grasses.</description><identifier>ISSN: 0021-8561</identifier><identifier>EISSN: 1520-5118</identifier><identifier>DOI: 10.1021/acs.jafc.6b02616</identifier><identifier>PMID: 27434508</identifier><language>eng</language><publisher>United States: American Chemical Society</publisher><subject>Alkaloids - chemistry ; Alkaloids - metabolism ; Chromatography, Liquid - methods ; Endophytes - metabolism ; Festuca - chemistry ; Festuca - microbiology ; Fungi - metabolism ; Lolium - chemistry ; Lolium - microbiology ; Poaceae - chemistry ; Poaceae - microbiology ; Tandem Mass Spectrometry - methods</subject><ispartof>Journal of agricultural and food chemistry, 2016-08, Vol.64 (31), p.6212-6218</ispartof><rights>Copyright © 2016 American Chemical Society</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-a336t-f1495c1a6e9d4a18b403ce60f10a5ac87931361dd3be315e428df7c71580f0a93</citedby><cites>FETCH-LOGICAL-a336t-f1495c1a6e9d4a18b403ce60f10a5ac87931361dd3be315e428df7c71580f0a93</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>314,780,784,27924,27925</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/27434508$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Adhikari, Khem B.</creatorcontrib><creatorcontrib>Boelt, Birte</creatorcontrib><creatorcontrib>Fomsgaard, Inge S.</creatorcontrib><title>Identification and Quantification of Loline-Type Alkaloids in Endophyte-Infected Grasses by LC-MS/MS</title><title>Journal of agricultural and food chemistry</title><addtitle>J. Agric. Food Chem</addtitle><description>Lolines, fungal metabolites of the grass–endophyte association, were identified and quantified using newly developed LC-MS/MS methods in endophyte-infected grasses belonging to the Lolium and Festuca genera after extraction with three different solvents using two extraction methods. The shaking extraction method with isopropanol/water was superior to the other methods due to its high sensitivity, high accuracy (recovery within or close to the range of 80–120%), and high precision (coefficient of variation of <10%). Seven loline alkaloids were identified and quantified using our newly established LC-MS/MS methods, and N-formylloline was the most abundant (5 mg/g dry matter), followed by N-acetylloline. These LC-MS/MS methods used the shortest sample handling time and the fewest sample preparation steps and proved to be good alternatives to existing GC and GC-MS analytical methods without compromising analytical efficiency. In conclusion, we developed for the first time a highly sensitive quantitative LC-MS/MS analytical method for the accurate and reproducible quantification and a LightSight-assisted LC-QTRAP/MS qualitative method for the tentative identification of loline-type alkaloids in endophyte-infected grasses.</description><subject>Alkaloids - chemistry</subject><subject>Alkaloids - metabolism</subject><subject>Chromatography, Liquid - methods</subject><subject>Endophytes - metabolism</subject><subject>Festuca - chemistry</subject><subject>Festuca - microbiology</subject><subject>Fungi - metabolism</subject><subject>Lolium - chemistry</subject><subject>Lolium - microbiology</subject><subject>Poaceae - chemistry</subject><subject>Poaceae - microbiology</subject><subject>Tandem Mass Spectrometry - methods</subject><issn>0021-8561</issn><issn>1520-5118</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2016</creationdate><recordtype>article</recordtype><recordid>eNp1kMFr2zAUh8XYWNJs956GjjvM6XuWJSvHEtI0kDJGu7ORpSfm1JEyyz7kv6-zZKWXngSP7_eBPsauEeYIOd4Ym-Y74-1c1ZArVB_YFGUOmUTUH9kURibTUuGEXaW0AwAtS_jMJnlZiEKCnjK3cRT6xjfW9E0M3ATHfw3m7Sl6vo1tEyh7Oh6I37bPpo2NS7wJfBVcPPw59pRtgifbk-PrzqREiddHvl1mD483D49f2Cdv2kRfL--M_b5bPS3vs-3P9WZ5u82MEKrPPBYLadEoWrjCoK4LEJYUeAQjjdXlQqBQ6JyoSaCkItfOl7ZEqcGDWYgZ-372Hrr4d6DUV_smWWpbEygOqUKNoJUqR--MwRm1XUypI18dumZvumOFUJ3aVmPb6tS2urQdJ98u9qHek3sd_I85Aj_OwL9pHLowfvZ93wvq74Sf</recordid><startdate>20160810</startdate><enddate>20160810</enddate><creator>Adhikari, Khem B.</creator><creator>Boelt, Birte</creator><creator>Fomsgaard, Inge S.</creator><general>American Chemical Society</general><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>7X8</scope></search><sort><creationdate>20160810</creationdate><title>Identification and Quantification of Loline-Type Alkaloids in Endophyte-Infected Grasses by LC-MS/MS</title><author>Adhikari, Khem B. ; Boelt, Birte ; Fomsgaard, Inge S.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-a336t-f1495c1a6e9d4a18b403ce60f10a5ac87931361dd3be315e428df7c71580f0a93</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2016</creationdate><topic>Alkaloids - chemistry</topic><topic>Alkaloids - metabolism</topic><topic>Chromatography, Liquid - methods</topic><topic>Endophytes - metabolism</topic><topic>Festuca - chemistry</topic><topic>Festuca - microbiology</topic><topic>Fungi - metabolism</topic><topic>Lolium - chemistry</topic><topic>Lolium - microbiology</topic><topic>Poaceae - chemistry</topic><topic>Poaceae - microbiology</topic><topic>Tandem Mass Spectrometry - methods</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Adhikari, Khem B.</creatorcontrib><creatorcontrib>Boelt, Birte</creatorcontrib><creatorcontrib>Fomsgaard, Inge S.</creatorcontrib><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><jtitle>Journal of agricultural and food chemistry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Adhikari, Khem B.</au><au>Boelt, Birte</au><au>Fomsgaard, Inge S.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Identification and Quantification of Loline-Type Alkaloids in Endophyte-Infected Grasses by LC-MS/MS</atitle><jtitle>Journal of agricultural and food chemistry</jtitle><addtitle>J. Agric. Food Chem</addtitle><date>2016-08-10</date><risdate>2016</risdate><volume>64</volume><issue>31</issue><spage>6212</spage><epage>6218</epage><pages>6212-6218</pages><issn>0021-8561</issn><eissn>1520-5118</eissn><abstract>Lolines, fungal metabolites of the grass–endophyte association, were identified and quantified using newly developed LC-MS/MS methods in endophyte-infected grasses belonging to the Lolium and Festuca genera after extraction with three different solvents using two extraction methods. The shaking extraction method with isopropanol/water was superior to the other methods due to its high sensitivity, high accuracy (recovery within or close to the range of 80–120%), and high precision (coefficient of variation of <10%). Seven loline alkaloids were identified and quantified using our newly established LC-MS/MS methods, and N-formylloline was the most abundant (5 mg/g dry matter), followed by N-acetylloline. These LC-MS/MS methods used the shortest sample handling time and the fewest sample preparation steps and proved to be good alternatives to existing GC and GC-MS analytical methods without compromising analytical efficiency. In conclusion, we developed for the first time a highly sensitive quantitative LC-MS/MS analytical method for the accurate and reproducible quantification and a LightSight-assisted LC-QTRAP/MS qualitative method for the tentative identification of loline-type alkaloids in endophyte-infected grasses.</abstract><cop>United States</cop><pub>American Chemical Society</pub><pmid>27434508</pmid><doi>10.1021/acs.jafc.6b02616</doi><tpages>7</tpages></addata></record> |
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subjects | Alkaloids - chemistry Alkaloids - metabolism Chromatography, Liquid - methods Endophytes - metabolism Festuca - chemistry Festuca - microbiology Fungi - metabolism Lolium - chemistry Lolium - microbiology Poaceae - chemistry Poaceae - microbiology Tandem Mass Spectrometry - methods |
title | Identification and Quantification of Loline-Type Alkaloids in Endophyte-Infected Grasses by LC-MS/MS |
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