{"id":43589,"date":"2020-10-28T00:00:00","date_gmt":"2020-10-28T00:00:00","guid":{"rendered":"https:\/\/discover.restek.com\/uncategorized\/schnelle-einfache-4-5-minuten-analyse-von-pyrrolizidinalkaloiden-mittels-lc-ms-ms\/"},"modified":"2025-11-13T23:32:58","modified_gmt":"2025-11-13T23:32:58","slug":"schnelle-einfache-4-5-minuten-analyse-von-pyrrolizidinalkaloiden-mittels-lc-ms-ms","status":"publish","type":"post","link":"https:\/\/discover.restek.com\/de\/artikel\/ffss3064-de\/schnelle-einfache-4-5-minuten-analyse-von-pyrrolizidinalkaloiden-mittels-lc-ms-ms","title":{"rendered":"Schnelle, einfache 4.5-Minuten-Analyse von Pyrrolizidinalkaloiden mittels LC-MS\/MS"},"content":{"rendered":"\n<ul class=\"wp-block-list\">\n<li>Schnelle 4.5-Minuten-Analyse von Pyrrolizidinalkaloiden erm\u00f6glicht Basislinientrennung der meisten Verbindungen.<\/li>\n\n\n\n<li>Analyten werden mit einer einfachen mobilen Phase und einem Gradienten schnell und mit sehr guter Peakform eluiert.<\/li>\n\n\n\n<li>Unter sauren Bedingungen liefert die robuste Raptor ARC-18 S\u00e4ule deutlich l\u00e4nger zuverl\u00e4ssige Ergebnisse als herk\u00f6mmliche C18-S\u00e4ulen.<\/li>\n<\/ul>\n\n\n\n<p>In der Natur kommen Pyrrolizidinalkaloide (PA) als sekund\u00e4re Stoffwechselprodukte in einer Vielzahl von Pflanzenarten vor (z. B. in G\u00e4nsebl\u00fcmchen, Vergissmeinnicht, H\u00fclsenfr\u00fcchten u. a.). Die toxischen Metabolite dienen der Pflanze zur Abwehr gegen Herbivoren und sind nach Angaben der Europ\u00e4ischen Beh\u00f6rde f\u00fcr Lebensmittelsicherheit (EFSA) vermutlich die am weitesten verbreiteten nat\u00fcrlichen Toxine. Pyrrolizidinalkaloide wurden in \u00fcber 6000 Pflanzenarten nachgewiesen, aber nur wenige Arten waren direkt an Vergiftungen von Menschen oder Tieren beteiligt. Unter den etwa 700 bekannten Pyrrolizidinalkaloiden gelten die 1,2-unges\u00e4ttigten Verbindungen als besonders toxisch, da sie t\u00f6dliche Leberfunktionsst\u00f6rungen verursachen k\u00f6nnen. Kr\u00e4uter, Tees, Honig und Getreide k\u00f6nnen mit Pyrrolizidinalkaloiden kontaminiert sein, wenn versehentlich Pflanzen mitgeerntet wurden, die diese Stoffe enthalten, oder diese als Nahrungsquelle f\u00fcr Honigbienen dienen.<\/p>\n\n\n\n<p>Aufgrund der Anwendung des ALARA-Prinzips (\u201eAs Low As Reasonably Achievable\u201c \u2013 so niedrig wie vern\u00fcnftig erreichbar) f\u00fcr Pyrrolizidinalkaloide durch die Codex-Alimentarius-Kommission der Weltgesundheitsorganisation (WHO) sowie vieler regionaler Bem\u00fchungen zur \u00dcberwachung dieser toxischen Stoffe in Nahrungs-, Futter- und Arzneimitteln, besteht ein zunehmender Bedarf f\u00fcr schnelle, pr\u00e4zise Methoden zur Analyse von Pyrrolizidinalkaloiden. Zur Zeit gibt es nur eine einzige harmonisierte Methode, die vom Deutschen Bundesinstitut f\u00fcr Risikobewertung (BfR) entwickelt und validiert wurde [1]. Sie verwendet einen Aufschluss mit Schwefels\u00e4ure, eine Aufreinigung durch Festphasenextraktion (SPE) an C18 und die Analyse mittels LC-MS\/MS. Die im BfR-Protokoll angegebene Beispielmethode verwendet eine 150 x 2.1 mm, 1.9 \u00b5m vollpor\u00f6se C18-S\u00e4ule &nbsp;und erzielt eine Analysezeit von 15 Minuten, wobei die letzte Verbindung, Lasiocarpin-N-oxid (LaN), bei 9.33 Minuten eluiert. In der nachfolgend beschriebenen Fallstudie ergab der Wechsel zu einer 50 x 2.1 mm, 2.7 \u00b5m Raptor ARC-18 Core-Shell S\u00e4ule &nbsp;ausreichende Retention und LaN eluierte in nur 3.2 Minuten (bei 4.5 Minuten Gesamtanalysezeit). Obwohl in diesem Beispiel ein UHPLC-Ger\u00e4t verwendet wurde, ist dies f\u00fcr eine solche Analyse nicht notwendig. Alle Substanzen eluieren mit sehr guter Peakform. Mit Ausnahme des Echimidins und des zugeh\u00f6rigen N-Oxids wiesen alle Verbindungen Basislinientrennung auf. Die spezielle Phasenchemie der Raptor ARC-18 S\u00e4ule f\u00fchrt unter sauren Bedingungen au\u00dferdem zu l\u00e4ngeren Standzeiten verglichen mit herk\u00f6mmlichen C18-S\u00e4ulen.<\/p>\n\n\n\n<p>Der st\u00e4ndig zunehmende Bedarf f\u00fcr Analysen von Pyrrolizidinalkaloiden erfordert auch die Entwicklung neuer Methoden. F\u00fcr die heutigen Herausforderungen k\u00f6nnen Laboratorien jedoch die Raptor ARC-18 S\u00e4ule nutzen, um ihre Methoden zu optimieren, die Gesamtanalysezeit zu verk\u00fcrzen und den Probendurchsatz zu erh\u00f6hen.<\/p>\n\n\n\n<h2 class=\"wp-block-heading\">Literatur<\/h2>\n\n\n\n<ol class=\"wp-block-list\">\n<li>Bundesinstitut f\u00fcr Risikobewertung (BfR), BfR-PA-Tee-2.0\/2014, Bestimmung von Pyrrolizidinalkaloiden (PA) in Pflanzenmaterial mittels SPE-LC-MS\/MS, 2014.&nbsp;<a href=\"https:\/\/www.bfr.bund.de\/cm\/343\/bestimmung-von-pyrrolizidinalkaloiden.pdf\" target=\"_blank\" rel=\"noreferrer noopener\">https:\/\/www.bfr.bund.de\/cm\/343\/bestimmung-von-pyrrolizidinalkaloiden.pdf<\/a><\/li>\n<\/ol>\n\n\n<div class=\"wp-block-custom-chromatogram-article-top\"><div class=\"chromatogram-article-placeholder\"><div class=\"figure-heading\"><\/div><div class='chromatogram-article-inner-full'><div class=\"chromatogram-article-inner\">\n<div class=\"wp-block-custom-chromatogram-article\"><div class=\"wp-block-custom-chromatogram-article\"><div class=\"chromatogram-image wide-image\"><img decoding=\"async\" src=\"https:\/\/ez.restek.com\/images\/cgram\/lc_ff0573.png\" alt=\"Pyrrolizidine Alkaloids on Raptor ARC-18 by LC-MS\/MS\" title=\"-\"><\/div><p class=\"article-id\" style=\"text-align:center\"> LC_FF0573<\/p><div class=\"chromatogram-peaks\"><h4>Peaks<\/h4><table class=\"peaks col-12\">\n<thead><tr><th><\/th><th style=\"text-align: left;width: 75px\">Peaks<\/th><th style=\"text-align: center;width: 75px\">t<sub>R<\/sub> (min)<\/th><th style=\"text-align: center;width: 75px\">Precursor<\/th><th style=\"text-align: center;width: 75px\">Product 1<\/th><th style=\"text-align: center;width: 75px\">Product 2<\/th><th style=\"text-align: center;width: 75px\">Product 3<\/th><\/tr><\/thead>\n<tbody><tr><td class=\"num\">1.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Monocrotaline\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/315-22-0\/Monocrotaline\" target=\"_blank\" rel=\"noopener\">Monocrotaline<\/a><\/td><td class=\"oth\">0.677<\/td><td class=\"oth\">326.20<\/td><td class=\"oth\">120.3<\/td><td class=\"oth\">121.30<\/td><td class=\"oth\">94.25<\/td><\/tr>\n<tr><td class=\"num\">2.<\/td><td class=\"cmpd\">Incidine<\/td><td class=\"oth\">1.111<\/td><td class=\"oth\">300.20<\/td><td class=\"oth\">94.15<\/td><td class=\"oth\">138.20<\/td><td class=\"oth\">156.36<\/td><\/tr>\n<tr><td class=\"num\">3.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Heliotrine\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/303-33-3\/Heliotrine\" target=\"_blank\" rel=\"noopener\">Heliotrine<\/a><\/td><td class=\"oth\">1.763<\/td><td class=\"oth\">314.30<\/td><td class=\"oth\">138.20<\/td><td class=\"oth\">156.20<\/td><td class=\"oth\">120.20<\/td><\/tr>\n<tr><td class=\"num\">4.<\/td><td class=\"cmpd\">Heliotrine N-oxide<\/td><td class=\"oth\">1.895<\/td><td class=\"oth\">330.25<\/td><td class=\"oth\">172.25<\/td><td class=\"oth\">138.20<\/td><td class=\"oth\"><\/td><\/tr>\n<tr><td class=\"num\">5.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Senecionine\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/130-01-8\/Senecionine\" target=\"_blank\" rel=\"noopener\">Senecionine<\/a><\/td><td class=\"oth\">2.240<\/td><td class=\"oth\">336.20<\/td><td class=\"oth\">120.30<\/td><td class=\"oth\">138.30<\/td><td class=\"oth\"><\/td><\/tr>\n<tr><td class=\"num\">6.<\/td><td class=\"cmpd\">Senecionine N-oxide<\/td><td class=\"oth\">2.410<\/td><td class=\"oth\">352.35<\/td><td class=\"oth\">94.20<\/td><td class=\"oth\">120.30<\/td><td class=\"oth\">118.25<\/td><\/tr>\n<tr><td class=\"num\">7.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Echimidine\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/520-68-3\/Echimidine\" target=\"_blank\" rel=\"noopener\">Echimidine<\/a><\/td><td class=\"oth\">2.524<\/td><td class=\"oth\">398.30<\/td><td class=\"oth\">120.25<\/td><td class=\"oth\">220.15<\/td><td class=\"oth\"><\/td><\/tr>\n<tr><td class=\"num\">8.<\/td><td class=\"cmpd\">Echimidine N-oxide<\/td><td class=\"oth\">2.528<\/td><td class=\"oth\">414.25<\/td><td class=\"oth\">396.30<\/td><td class=\"oth\">352.20<\/td><td class=\"oth\">254.25<\/td><\/tr>\n<tr><td class=\"num\">9.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Lasiocarpine\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/303-34-4\/Lasiocarpine\" target=\"_blank\" rel=\"noopener\">Lasiocarpine<\/a><\/td><td class=\"oth\">3.028<\/td><td class=\"oth\">412.20<\/td><td class=\"oth\">120.20<\/td><td class=\"oth\">220.15<\/td><td class=\"oth\">336.25<\/td><\/tr>\n<tr><td class=\"num\">10.<\/td><td class=\"cmpd\">Lasiocarpine N-oxide<\/td><td class=\"oth\">3.260<\/td><td class=\"oth\">428.25<\/td><td class=\"oth\">254.25<\/td><td class=\"oth\">352.25<\/td><td class=\"oth\">120.30<\/td><\/tr>\n<\/tbody><\/table><\/div><div class=\"chromatogram-conditions\"><h4>Conditions<\/h4><div class=\"conditions-container container-fluid\"><div class=\"row\"><table class=\"conditions col-lg-6 col-12\"><tr><th class=\"conditions_header\" scope=\"row\">Column<\/th><td>Raptor ARC-18  (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/9314A52?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=LC_FF0573\" rel=\"noopener\">cat.# 9314A52<\/a>)<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Dimensions:<\/th><td>50 mm x 2.1 mm ID<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Particle Size:<\/th><td>2.7 \u00b5m<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Pore Size:<\/th><td>90 \u00c5<\/td><\/tr><tr><td><\/td><tr><th class=\"sub conditions_header\" scope=\"row\">Temp.:<\/th><td>25 \u00b0C<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Standard\/Sample<\/th><td><\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Diluent:<\/th><td>0.1% Formic acid in water<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Conc.:<\/th><td>10 ng\/mL<\/td><\/tr><td><\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Inj. Vol.:<\/th><td>1 \u00b5L <\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Mobile Phase<\/th><td><\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">A:<\/th><td>0.1% Formic acid in water <\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">B:<\/th><td>0.1% Formic acid in acetonitrile <\/td><\/tr><tr><td><\/td><td><table class=\"cgram_ramp\"><thead><tr><th>Time (min)<\/th><th>Flow (mL\/min)<\/th><th>%A<\/th><th>%B<\/th><\/tr><\/thead><tbody><tr><td>0.00<\/td><td>0.5<\/td><td>95<\/td><td>5<\/td><\/tr><tr><td>3.5<\/td><td>0.5<\/td><td>65<\/td><td>35<\/td><\/tr><tr><td>3.51<\/td><td>0.5<\/td><td>95<\/td><td>5<\/td><\/tr><tr><td>4.5<\/td><td>0.5<\/td><td>95<\/td><td>5<\/td><\/tr><\/tbody><\/table><\/td><\/tr><\/table><table class=\"conditions col-lg-6 col-12\"><tr><th class=\"conditions_header\" scope=\"row\">Detector<\/th><td>MS\/MS<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Ion Mode:<\/th><td>ESI+ <\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Instrument<\/th><td>UHPLC<\/td><\/tr><\/table><\/div><\/div><\/div><div class=\"chromatogram-pdf-link\"><a href=\"https:\/\/ez.restek.com\/images\/cgram\/lc_ff0573.pdf\" target=\"_blank\" rel=\"noopener noreferrer\"><svg xmlns=\"http:\/\/www.w3.org\/2000\/svg\" width=\"18\" height=\"18\" viewBox=\"0 0 18 18\"><g data-name=\"Group 2996\"><path data-name=\"Rectangle 1246\" d=\"M0 0h18v18H0z\" style=\"fill: none;\"><\/path><\/g><g data-name=\"Group 2997\"><path data-name=\"Path 729\" d=\"M13.412 11.4v2.017H5.345V11.4H4v2.017a1.349 1.349 0 0 0 1.345 1.345h8.068a1.349 1.349 0 0 0 1.345-1.345V11.4zm-.672-2.694-.948-.948-1.741 1.735V4H8.706v5.493L6.965 7.758l-.948.948 3.361 3.361z\" transform=\"translate(-.437 -.414)\" style=\"fill: rgb(13, 123, 196);\"><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n<\/div><\/div><\/div>\n\n\n<div style=\"height:100px\" aria-hidden=\"true\" class=\"wp-block-spacer\"><\/div>\n","protected":false},"excerpt":{"rendered":"<p>Die Analyse von Pyrrolizidinalkaloiden ist mit einer typischen Laufzeit von 15 Minuten zeitaufw\u00e4ndig, und der Schritt des S\u00e4ureaufschlusses kann die Lebensdauer der analytischen S\u00e4ule verk\u00fcrzen. Im Gegensatz dazu eluiert bei dieser Analyse mit einer s\u00e4urebest\u00e4ndigen Raptor ARC-18-S\u00e4ule die letzte Verbindung in nur 3.2 Minuten mit guter Peakform und Trennung.<\/p>\n","protected":false},"author":11,"featured_media":6937,"comment_status":"closed","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"_acf_changed":false,"_kad_blocks_custom_css":"","_kad_blocks_head_custom_js":"","_kad_blocks_body_custom_js":"","_kad_blocks_footer_custom_js":"","_kadence_starter_templates_imported_post":false,"_kad_post_transparent":"","_kad_post_title":"","_kad_post_layout":"","_kad_post_sidebar_id":"","_kad_post_content_style":"","_kad_post_vertical_padding":"","_kad_post_feature":"","_kad_post_feature_position":"","_kad_post_header":false,"_kad_post_footer":false,"footnotes":""},"categories":[787],"tags":[],"industries-application":[2236,2238],"post-badge":[],"resource-type":[],"product-library":[2481,2499],"resource-technique":[2326,2299,2328,2363],"ppma_author":[414],"class_list":["post-43589","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-artikel","industries-application-lebensmittel-getranke","industries-application-lebensmittelsicherheit","product-library-flussigchromatographie-produkte","product-library-lc-saulen","resource-technique-flussigchromatografie","resource-technique-liquid-chromatography","resource-technique-massenspektrometrie-ms","resource-technique-ms-ms-de"],"acf":[],"taxonomy_info":{"category":[{"value":787,"label":"Artikel"}],"industries-application":[{"value":2236,"label":"Lebensmittel &amp; 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