{"id":43590,"date":"2020-10-28T00:00:00","date_gmt":"2020-10-28T00:00:00","guid":{"rendered":"https:\/\/discover.restek.com\/uncategorized\/analyse-simple-et-rapide-des-alcaloides-pyrrolizidiniques-en-4-5-minutes-sur-colonne-lc-msms-raptor-arc-18\/"},"modified":"2026-01-28T19:18:14","modified_gmt":"2026-01-28T19:18:14","slug":"analyse-simple-et-rapide-des-alcaloides-pyrrolizidiniques-en-4-5-minutes-sur-colonne-lc-msms-raptor-arc-18","status":"publish","type":"post","link":"https:\/\/discover.restek.com\/fr\/articles-fr\/ffss3064-fr\/analyse-simple-et-rapide-des-alcaloides-pyrrolizidiniques-en-4-5-minutes-sur-colonne-lc-msms-raptor-arc-18","title":{"rendered":"Analyse simple et rapide des alcalo\u00efdes pyrrolizidiniques en 4.5 minutes sur colonne LC-MS\/MS Raptor ARC-18"},"content":{"rendered":"\n<ul class=\"wp-block-list\">\n<li>Analyse rapide des alcalo\u00efdes pyrrolizidiniques en 4.5 minutes permettant de s\u00e9parer la plupart des compos\u00e9s \u00e0 la ligne de base.<\/li>\n\n\n\n<li>Phase mobile simple et gradient permettant l\u2019\u00e9lution rapide des compos\u00e9s avec une excellente forme de pic.<\/li>\n\n\n\n<li>La colonne Raptor ARC-18 est r\u00e9sistante et sa dur\u00e9e de vie est sup\u00e9rieure \u00e0 celle des colonnes C18 classiques en milieu acide.<\/li>\n<\/ul>\n\n\n\n<p>Les alcalo\u00efdes pyrrolizidiniques (AP) sont des toxines naturellement pr\u00e9sentes dans une grande vari\u00e9t\u00e9 d\u2019esp\u00e8ces v\u00e9g\u00e9tales (par exemple, les marguerites, les myosotis et les l\u00e9gumineuses, entre autres). Ce sont des m\u00e9tabolites secondaires qui se forment pour prot\u00e9ger les plantes des herbivores et, d&#8217;apr\u00e8s l\u2019EFSA (Autorit\u00e9 europ\u00e9enne de s\u00e9curit\u00e9 des aliments), elles sont probablement les toxines naturelles les plus largement distribu\u00e9es. Il existe plus de 6 000 esp\u00e8ces v\u00e9g\u00e9tales connues contentant des alcalo\u00efdes pyrrolizidiniques, mais seules quelques unes ont \u00e9t\u00e9 directement impliqu\u00e9es dans l\u2019empoisonnement d\u2019\u00eatres humains ou d\u2019animaux. De plus, parmi environ 700 AP connus, les compos\u00e9s 1,2-insatur\u00e9s ont \u00e9t\u00e9 identifi\u00e9s comme les plus toxiques, capables de provoquer des l\u00e9sions h\u00e9patiques mortelles. Les herbes aromatiques et m\u00e9dicinales, les th\u00e9s et les c\u00e9r\u00e9ales peuvent \u00eatre contamin\u00e9s par des alcalo\u00efdes pyrrolizidiniques si des plantes contenant des AP sont accidentellement r\u00e9colt\u00e9es en m\u00eame temps, ou utilis\u00e9es pour nourrir les abeilles.<\/p>\n\n\n\n<p>La Commission du Codex Alimentarius de l\u2019Organisation mondiale de la sant\u00e9 (OMS) a adopt\u00e9 le principe ALARA (principe du niveau de risque le plus bas que l&#8217;on peut raisonnablement atteindre) pour les AP, et de nombreux efforts locaux visent \u00e0 surveiller ces compos\u00e9s toxiques dans l\u2019alimentation, le fourrage et les m\u00e9dicaments. La demande de m\u00e9thodes d\u2019analyse rapides et pr\u00e9cises pour les alcalo\u00efdes pyrrolizidiniques est donc en pleine augmentation. Actuellement, la seule m\u00e9thode harmonis\u00e9e a \u00e9t\u00e9 mise au point et valid\u00e9e par l\u2019institut f\u00e9d\u00e9ral allemand d&#8217;\u00e9valuation des risques (BfR) [1]. Elle fait intervenir une digestion \u00e0 l\u2019acide sulfurique, une SPE sur colonne C18 et une analyse par LC-MS\/MS. L\u2019exemple de m\u00e9thode fourni par le protocole du BfR utilise un colonne C18 \u00e0 particules de 1,9 \u03bcm enti\u00e8rement poreuses mesurant 150 x 2,1 mm, et il produit une analyse de 15 minutes o\u00f9 le dernier composant, le lasiocarpine-N-oxyde (LaN) est \u00e9lu\u00e9 \u00e0 9.33 minutes. En revanche, dans le cas \u00e9tudi\u00e9 ici, le passage \u00e0 une colonne Raptor ARC-18 de 50 x 2,1 mm avec particules silice de 2,7 \u03bcm superficiellement poreuses fournit une r\u00e9tention suffisante et une \u00e9lution du LaN en 3.2 minutes seulement (soit 4.5 minutes d\u2019analyse au total). Il convient de noter qu\u2019un instrument UHPLC a \u00e9t\u00e9 utilis\u00e9 dans cet exemple, mais qu\u2019il n\u2019est pas n\u00e9cessaire pour cette analyse. D\u2019excellentes formes de pics ont \u00e9t\u00e9 obtenues et tous les compos\u00e9s, sauf l\u2019\u00e9chimidine et le N-oxyde correspondant, ont \u00e9t\u00e9 \u00e9lu\u00e9s \u00e0 la ligne de base. La composition chimique unique de la phase de la colonne Raptor ARC-18 fournit \u00e9galement une dur\u00e9e de vie plus longue en milieu acide, par rapport aux colonnes C18 classiques.<\/p>\n\n\n\n<p>\u00c0 mesure que la port\u00e9e des analyses des alcalo\u00efdes pyrrolizidiniques continue de s&#8217;\u00e9largir, les m\u00e9thodes vont devoir \u00e9voluer \u00e9galement. Mais pour les difficult\u00e9s d\u2019aujourd\u2019hui, l\u2019utilisation d\u2019une colonne Raptor ARC-18 permet aux laboratoires d\u2019optimiser les conditions de leurs m\u00e9thodes, de raccourcir la dur\u00e9e des analyses et d\u2019am\u00e9liorer la cadence de traitement.<\/p>\n\n\n\n<div style=\"height:20px\" aria-hidden=\"true\" class=\"wp-block-spacer\"><\/div>\n\n\n\n<h2 class=\"wp-block-heading\">R\u00e9f\u00e9rences<\/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.\u00a0<a href=\"https:\/\/www.bfr.bund.de\/cm\/343\/bestimmung-von-pyrrolizidinalkaloiden.pdf\" target=\"_blank\" rel=\"noopener\"><strong>https:\/\/www.bfr.bund.de\/cm\/343\/bestimmung-von-pyrrolizidinalkaloiden.pdf<\/strong><\/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>La consommation grandissante d\u2019alcalo\u00efdes pyrrolizidiniques inqui\u00e8te de plus en plus les pays de l\u2019UE, les obligeant \u00e0 diligenter des travaux de surveillance. Bien que la liste des analytes ne soit pas encore d\u00e9finitive, Restek a mis au point une m\u00e9thode LC-MS\/MS simple et rapide pour aider les laboratoires qui doivent d\u00e9velopper cette analyse.<\/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":[462],"tags":[],"industries-application":[2214,2216],"post-badge":[],"resource-type":[],"product-library":[2463,2445],"resource-technique":[2318,2362,2320],"ppma_author":[414],"class_list":["post-43590","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-articles-fr","industries-application-industrie-agroalimentaire","industries-application-securite-alimentaire","product-library-colonnes-lc","product-library-produits-pour-la-chromatographie-en-phase-liquide","resource-technique-chromatographie-en-phase-liquide","resource-technique-ms-ms-fr","resource-technique-spectrometrie-de-masse-ms"],"acf":[],"taxonomy_info":{"category":[{"value":462,"label":"Articles"}],"industries-application":[{"value":2214,"label":"Industrie 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