{"id":43585,"date":"2020-10-23T01:00:00","date_gmt":"2020-10-23T01:00:00","guid":{"rendered":"https:\/\/discover.restek.com\/uncategorized\/analyse-plus-rapide-du-3-mcpd-et-des-esters-glycidyliques-en-gc-ms-dans-les-huiles-comestibles-sur-la-colonne-rxi-17sil-ms\/"},"modified":"2025-12-16T13:42:58","modified_gmt":"2025-12-16T13:42:58","slug":"analyse-plus-rapide-du-3-mcpd-et-des-esters-glycidyliques-en-gc-ms-dans-les-huiles-comestibles-sur-la-colonne-rxi-17sil-ms","status":"publish","type":"post","link":"https:\/\/discover.restek.com\/fr\/articles-fr\/ffss3027-fr\/analyse-plus-rapide-du-3-mcpd-et-des-esters-glycidyliques-en-gc-ms-dans-les-huiles-comestibles-sur-la-colonne-rxi-17sil-ms","title":{"rendered":"Analyse plus rapide du 3-MCPD et des esters glycidyliques en GC-MS dans les huiles comestibles sur la colonne Rxi-17Sil MS"},"content":{"rendered":"\n<ul class=\"wp-block-list\">\n<li>Conforme aux exigences de la m\u00e9thode AOS Cd 29c-13 &#8211; Conditions analytiques optimis\u00e9e.<\/li>\n\n\n\n<li>L\u2019injection &#8220;split&#8221; r\u00e9duit la dur\u00e9e de l\u2019analyse de 8 min et att\u00e9nue les dommages provoqu\u00e9s par les r\u00e9actifs de d\u00e9rivatisation.<\/li>\n\n\n\n<li>Plus de souplesse : injection PTV ou &#8220;split\/splitless&#8221;.<\/li>\n<\/ul>\n\n\n\n<p>Les esters d\u2019acides gras du 3-chloropropane-1,2,-diol (3-MCPD) et les esters glycidyliques pr\u00e9sents dans les huiles comestibles sont des contaminants form\u00e9s pendant le raffinage. \u00c0 l\u2019ingestion, ces compos\u00e9s d\u00e9gagent du MCPD et du glycidol sous forme libre, consid\u00e9r\u00e9s comme potentiellement canc\u00e9rig\u00e8nes et\/ou g\u00e9notoxiques. L\u2019approche analytique la plus courante est une m\u00e9thode indirecte o\u00f9 les esters de l\u2019\u00e9chantillon sont hydrolys\u00e9s, d\u00e9rivatis\u00e9s \u00e0 nouveau, puis analys\u00e9s par GC-MS. Les m\u00e9thodes comme la m\u00e9thode AOS Cd 29c-13 (ou un \u00e9quivalent international (ISO 18363-1) ou national (DGF C-VI 18 (10)) sont habituellement utilis\u00e9es pour cette analyse. Pendant le processus de pr\u00e9paration des \u00e9chantillons, le glycidol libre est transform\u00e9 en 3-MCPD en conditions acides, puis il est analys\u00e9 avec le 3-MCPD form\u00e9 directement. La m\u00e9thode par chromatographie exige un injecteur PTV utilis\u00e9 en mode &#8220;splitless&#8221;, ce qui n\u00e9cessite une temp\u00e9rature du four basse (85\u00b0C) au d\u00e9part et un effet de solvant pour maintenir des pics sym\u00e9triques, surtout pour les compos\u00e9s rapidement \u00e9lu\u00e9s. Apr\u00e8s plusieurs gradients de temp\u00e9rature, la dur\u00e9e finale de l\u2019analyse (conform\u00e9ment \u00e0 la m\u00e9thode AOS Cd 29c-13) est de moins de 25 minutes.<\/p>\n\n\n\n<p>Pour proposer aux laboratoires une m\u00e9thode d\u2019analyse du 3-MCPD et des esters glycidyliques moins chronophage, nous avons optimis\u00e9 la technique d\u2019injection de l&#8217;\u00e9chantillon et le programme de temp\u00e9rature de la m\u00e9thode AOS Cd 29c-13. Nous sommes pass\u00e9s tout d\u2019abord \u00e0 une injection &#8220;split&#8221; car elle r\u00e9duit la quantit\u00e9 de r\u00e9actif de d\u00e9rivatisation qui p\u00e9n\u00e8tre dans le syst\u00e8me. Cette m\u00e9thode est moins agressive pour la colonne et pour le GC-MS et permet de r\u00e9duire les co\u00fbts et la fr\u00e9quence des maintenances. En outre, le transfert de l\u2019\u00e9chantillon de l\u2019injecteur dans la colonne \u00e9tant bien plus rapide en mode &#8220;split&#8221; qu\u2019en mode &#8220;splitless&#8221;, l\u2019effet solvant est moins n\u00e9cessaire et la temp\u00e9rature initiale du four peut \u00eatre sensiblement plus \u00e9lev\u00e9e. L\u2019augmentation de la temp\u00e9rature de d\u00e9part du four \u00e0 120 \u030aC a produit des pics fins et, m\u00eame avec un rapport de division de 10:1, les limites de d\u00e9tection \u00e9taient convenables. Le fait de doubler la vitesse de mont\u00e9e en temp\u00e9rature de 6\u00b0C\/min \u00e0 12 \u030aC\/min a aussi consid\u00e9rablement acc\u00e9l\u00e9r\u00e9 l\u2019analyse sans effet n\u00e9gatif. La temp\u00e9rature finale du four \u00e9tait \u00e9galement plus \u00e9lev\u00e9e afin d&#8217;\u00e9liminer plus efficacement les contaminants \u00e0 haut poids mol\u00e9culaire de la colonne. La m\u00e9thode optimis\u00e9e pr\u00e9sent\u00e9e ici a fait gagner 8 minutes par rapport \u00e0 la dur\u00e9e de l\u2019analyse AOS Cd 29c-13 et pr\u00e9sentait de bonnes performances, aussi bien avec les injecteurs PTV qu\u2019avec des injecteurs &#8220;split\/splitless&#8221; d\u00e9di\u00e9s. Elle permet d\u2019obtenir des analyses plus rapides et une plus grande souplesse pour les laboratoires qui analysent le 3-MCPD et les esters glycidyliques dans les huiles comestibles.<\/p>\n\n\n<div class=\"wp-block-custom-chromatogram-article-top\"><div class=\"wp-block-custom-chromatogram-article\"><div class='chromatogram-article-inner-full'><div class=\"chromatogram-image wide-image\"><img decoding=\"async\" src=\"https:\/\/ez.restek.com\/images\/cgram\/gc_fs0566.png\" alt=\"3-Monochloropropane-1,2-Diol (3-MCPD) Esters in Olive Oil on Rxi-17Sil MS\" title=\"-\"><\/div><p class=\"article-id\" style=\"text-align:center\"> GC_FS0566<\/p><div class=\"chromatogram-peaks\"><h4>Peaks<\/h4><table class=\"peaks col-lg-6 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\">Conc.<br \/>(ng\/mL)<\/th><\/tr><\/thead>\n<tbody><tr><td class=\"num\">1.<\/td><td class=\"cmpd\">3-MCPD-d5 PBA derivative<\/td><td class=\"oth\">5.937<\/td><td class=\"oth\">1.81<\/td><\/tr>\n<tr><td class=\"num\">2.<\/td><td class=\"cmpd\">3-MCPD PBA derivative<\/td><td class=\"oth\">5.977<\/td><td class=\"oth\">2.94<\/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>Rxi-17Sil MS, 30 m, 0.25 mm ID, 0.25 \u00b5m (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/14123?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=GC_FS0566\" rel=\"noopener\">cat.# 14123<\/a>)<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Standard\/Sample<\/th><td>Extracted olive oil<\/td><\/tr>\n<tr><th class=\"sub conditions_header\" scope=\"row\">Diluent:<\/th><td>Isooctane<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Injection<\/th><td><\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Inj. Vol.:<\/th><td>1 \u00b5L split (split ratio 10:1)<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Liner:<\/th><td>Topaz 4.0 mm ID Precision inlet liner w\/wool (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/23305?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=GC_FS0566\" rel=\"noopener\">cat.# 23305<\/a>)<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Inj. Temp.:<\/th><td>280 \u00b0C<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\" colspan=\"2\">Oven<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Oven Temp.:<\/th><td>120 &#176;C (hold 0.5 min) to 180 &#176;C at 12 &#176;C\/min to 330 &#176;C at 25 &#176;C\/min (hold 5 min)<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Carrier Gas<\/th><td>He, constant flow<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Flow Rate:<\/th><td>1.4 mL\/min<\/td><\/tr><\/table><table class=\"conditions col-lg-6 col-12\"><tr><th class=\"conditions_header\" scope=\"row\">Detector<\/th><td>MS<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Mode:<\/th><td>SIM<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">SIM Program:<\/th><td colspan=\"2\">147, 150, 196, 201 m\/z, 50 ms dwell<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Transfer Line Temp.:<\/th><td>320 \u00b0C<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Analyzer Type:<\/th><td>Quadrupole <\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Source Temp.:<\/th><td>230 \u00b0C<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Quad Temp.:<\/th><td>150 \u00b0C<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Instrument<\/th><td>Agilent 7890A GC &amp; 5975C MSD<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Sample Preparation<\/th><td>The olive oil sample was spiked with 3-MCPD-d5 ester and prepared according to AOCS method Cd 29c-13.<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Notes<\/th><td>Restek MCPD reference standards are now available. Search for MCPD on www.restek.com to view our full selection.<\/td><\/tr><\/table><\/div><\/div><\/div><div class=\"chromatogram-pdf-link\"><a href=\"https:\/\/ez.restek.com\/images\/cgram\/gc_fs0566.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\n\n<div style=\"height:100px\" aria-hidden=\"true\" class=\"wp-block-spacer\"><\/div>\n","protected":false},"excerpt":{"rendered":"<p>L&#8217;analyse du 3-MCPD et des esters glycidyliques selon la m\u00e9thode AOCS Cd 29c-13 est chronophage et expose le GC-MS \u00e0 des r\u00e9actifs de d\u00e9rivatisation agressifs qui peuvent limiter la dur\u00e9e de vie de la colonne et augmenter les co\u00fbts de maintenance. Ici, nous avons optimis\u00e9 la m\u00e9thode en utilisant l&#8217;injection \u00ab Split \u00bb, ce qui permet de gagner 8 minutes, de r\u00e9duire les dommages caus\u00e9s par les r\u00e9actifs de d\u00e9rivatisation et d&#8217;utiliser des injecteurs PTV ou des injecteurs Split\/Splitless&#8221;.&#8221;<\/p>\n","protected":false},"author":11,"featured_media":6931,"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":[2456,2443,2446,2452,2458,2444],"resource-technique":[2316,2320],"hf_cat_post":[650],"ppma_author":[414],"class_list":["post-43585","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-gc","product-library-echantillonnage-dair-et-de-gaz","product-library-etalons-de-reference","product-library-etalons-gazeux-accessoires","product-library-pieces-de-rechange-pour-injecteur","product-library-produits-pour-la-chromatographie-en-phase-gazeuse","resource-technique-chromatographie-en-phase-gazeuse-gc","resource-technique-spectrometrie-de-masse-ms"],"acf":[],"taxonomy_info":{"category":[{"value":462,"label":"Articles"}],"industries-application":[{"value":2214,"label":"Industrie 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