{"id":76488,"date":"2022-08-24T00:00:00","date_gmt":"2022-08-24T00:00:00","guid":{"rendered":"https:\/\/discover.restek.com\/?p=76488"},"modified":"2026-01-28T21:48:37","modified_gmt":"2026-01-28T21:48:37","slug":"separation-amelioree-de-l-indeno123-cdpyrene-et-du-dibenzahanthracene-sur-la-nouvelle-colonne-rxi-svocms","status":"publish","type":"post","link":"https:\/\/discover.restek.com\/fr\/blog-fr\/gnbl5506-fr\/separation-amelioree-de-l-indeno123-cdpyrene-et-du-dibenzahanthracene-sur-la-nouvelle-colonne-rxi-svocms","title":{"rendered":"S\u00e9paration am\u00e9lior\u00e9e de l\u2019ind\u00e9no(1,2,3-c,d)pyr\u00e8ne et du dibenz[a,h]anthrac\u00e8ne sur la nouvelle colonne Rxi-SVOCms"},"content":{"rendered":"\n<p>Lors du d\u00e9veloppement de la colonne Rxi-SVOCms, notre objectif \u00e9tait d\u2019optimiser la r\u00e9solution des HAP isobares tout en visant un temps de r\u00e9tention de 16 minutes pour le benzo[ghi]p\u00e9ryl\u00e8ne (<strong>BghiP<\/strong>) sur une colonne de 30 m x 0,25 mm x 0,25 \u00b5m en utilisant nos param\u00e8tres d\u2019acquisition des COSV en injection &#8220;split&#8221; [<a href=\"https:\/\/fr.restek.com\/chromatogram-detail\/GC_EV1604\" data-type=\"link\" data-id=\"https:\/\/fr.restek.com\/chromatogram-detail\/GC_EV1604\" target=\"_blank\" rel=\"noopener\">GC_EV1604<\/a>]. La s\u00e9paration benzo[b]fluoranthene &#8211; benzo[k]fluoranthene (<strong>BbF &#8211; BkF<\/strong>) est celle qui demande le plus d&#8217;attention, mais nous avons \u00e9galement consacr\u00e9 de nombreuses ressources pour optimiser celle de l\u2019ind\u00e9no[123-cd]pyr\u00e8ne et le dibenz[ah]anthrac\u00e8ne (<strong>IcdP &#8211; DahA<\/strong>) dans le temps imparti.<\/p>\n\n\n<style>.kb-image76488_e0e686-7d .kb-image-has-overlay:after{opacity:0.3;}<\/style>\n<figure class=\"wp-block-kadence-image kb-image76488_e0e686-7d size-full\"><img loading=\"lazy\" decoding=\"async\" width=\"398\" height=\"667\" src=\"https:\/\/discover.restek.com\/wp-content\/uploads\/blog-improved-indeno-123-cd-pyrene-dibenz-ah-anthracene-separation-on-the-new-RXI-SVOCMS-column-01.png\" alt=\"\" class=\"kb-img wp-image-78091\" title=\"-\" srcset=\"https:\/\/discover.restek.com\/wp-content\/uploads\/blog-improved-indeno-123-cd-pyrene-dibenz-ah-anthracene-separation-on-the-new-RXI-SVOCMS-column-01.png 398w, https:\/\/discover.restek.com\/wp-content\/uploads\/blog-improved-indeno-123-cd-pyrene-dibenz-ah-anthracene-separation-on-the-new-RXI-SVOCMS-column-01-179x300.png 179w\" sizes=\"auto, (max-width: 398px) 100vw, 398px\" \/><\/figure>\n\n\n\n<p><\/p>\n\n\n\n<p><em>Figure 1 &#8211; Chromatogramme des ions caract\u00e9ristiques (m\/z) d\u2019ind\u00e9no[123-cd]pyr\u00e8ne (\u00e0 gauche), montrant une bonne s\u00e9paration des interf\u00e9rences de dibenz[ah]anthrac\u00e8ne (\u00e0 droite). Les sommets repr\u00e9sentent les aires de pics pour le [276+].<\/em><\/p>\n\n\n\n<p>Pourquoi ces deux HAP dont les masses molaires sont diff\u00e9rentes doivent \u00eatre s\u00e9par\u00e9s par la chromatographie ? Parce que le <strong>DahA <\/strong>(masse molaire = 278 g\/mol) g\u00e9n\u00e8re un signal tr\u00e8s fort \u00e0 m\/z = 276 (la masse molaire de l\u2019<strong>IcdP<\/strong>) sous une ionisation \u00e9lectronique \u00e0 70eV. La co\u00e9lution de ces deux compos\u00e9s entra\u00eene plusieurs probl\u00e8mes lors de l\u2019analyse :<\/p>\n\n\n\n<ul class=\"wp-block-list\">\n<li>Biais d&#8217;\u00e9talonnage<\/li>\n\n\n\n<li>Mauvaise caract\u00e9risation de la toxicit\u00e9 de l\u2019\u00e9chantillon<\/li>\n\n\n\n<li>Identification erron\u00e9e du signal de <strong>DahA <\/strong>[276+] comme celui de l&#8217;<strong>IcdP <\/strong>(particuli\u00e8rement probl\u00e9matique pour les essais d\u2019aptitude)<\/li>\n<\/ul>\n\n\n\n<h2 class=\"wp-block-heading\">Biais d&#8217;\u00e9talonnage<\/h2>\n\n\n\n<p>La Figure 1 repr\u00e9sente un chromatogramme des ions extraits (XIC ; Extracted ion Chromatogram) pour l\u2019<strong>IcdP <\/strong>o\u00f9 l\u2019<strong>IcdP <\/strong>et le <strong>DahA <\/strong>sont bien s\u00e9par\u00e9s avec la colonne<strong> Rxi-SVOCms<\/strong> (<a href=\"https:\/\/fr.restek.com\/p\/16623\" data-type=\"link\" data-id=\"https:\/\/fr.restek.com\/p\/16623\" target=\"_blank\" rel=\"noopener\">r\u00e9f.16623<\/a>). Si l\u2019<strong>IcdP <\/strong>et le <strong>DahA <\/strong>co\u00e9luaient, le signal de l\u2019ion quantitatif ([276+]) de l\u2019<strong>IcdP <\/strong>augmenterait de 38,2 % du fait des ions de <strong>DahA<\/strong>. Un \u00e9talonnage r\u00e9alis\u00e9 dans ces conditions entra\u00eenerait un biais n\u00e9gatif important dans la concentration d\u2019<strong>IcdP <\/strong>calcul\u00e9e dans un extrait d&#8217;\u00e9chantillon.<\/p>\n\n\n\n<h2 class=\"wp-block-heading\">Mauvaise caract\u00e9risation de la toxicit\u00e9 de l\u2019\u00e9chantillon<\/h2>\n\n\n\n<p>Le profil toxicologique d\u2019un m\u00e9lange de HAP se caract\u00e9rise par des facteurs d\u2019\u00e9quivalence (<strong>PEF<\/strong>, Potency Equivalency Factor). La carcinog\u00e9nicit\u00e9 est exprim\u00e9e par rapport au compos\u00e9 de r\u00e9f\u00e9rences &#8220;Benzo[a]pyr\u00e8ne (BaP)&#8221; :<\/p>\n\n\n\n<ul class=\"wp-block-list\">\n<li>Ind\u00e9no[123-cd]pyr\u00e8ne PEF = 0.1<\/li>\n\n\n\n<li>Dibenz[ah]anthrac\u00e8ne PEF = 2.4<\/li>\n\n\n\n<li>Benzo[b]fluoranth\u00e8ne PEF = 0.1<\/li>\n\n\n\n<li>Benzo[k]fluoranth\u00e8ne PEF = 0.1<\/li>\n\n\n\n<li>Benzo[a]pyr\u00e8ne PEF = 1.0<\/li>\n<\/ul>\n\n\n\n<p>Le PEF de l\u2019<strong>IcdP <\/strong>est de 0,1 seulement, tandis que celui du <strong>DahA <\/strong>est de 2,4. Donc, le fait de rapporter une concentration d\u2019<strong>IcdP <\/strong>dans les \u00e9chantillons avec un biais n\u00e9gatif de 40 % ne devrait pas \u00eatre si grave, n\u2019est-ce pas ? La r\u00e9ponse d\u00e9pend vraiment de la quantit\u00e9 relative de chaque HAP dans les \u00e9chantillons. La Figure 2 repr\u00e9sente le r\u00e9sultat d\u2019analyse du m\u00e9lange de goudrons de houille de HAP, NIST SRM. Dans ce cas, la contamination par l\u2019<strong>IcdP <\/strong>d\u00e9passe largement le <strong>DahA<\/strong>. S\u2019il s\u2019agissait d\u2019un analyse des HAP dans une matrice alimentaire, un biais de 40 % en moins dans la valeur calcul\u00e9e pour un HAP associ\u00e9 \u00e0 un signal fort pourra faire la diff\u00e9rence entre un aliment caract\u00e9ris\u00e9 comme dangereux pour les \u00eatres humains et un faux n\u00e9gatif permettant la distribution du produit.<\/p>\n\n\n<style>.kb-image76488_9490f8-84 .kb-image-has-overlay:after{opacity:0.3;}<\/style>\n<figure class=\"wp-block-kadence-image kb-image76488_9490f8-84 size-full\"><img loading=\"lazy\" decoding=\"async\" width=\"505\" height=\"678\" src=\"https:\/\/discover.restek.com\/wp-content\/uploads\/blog-improved-indeno-123-cd-pyrene-dibenz-ah-anthracene-separation-on-the-new-RXI-SVOCMS-column-02.png\" alt=\"\" class=\"kb-img wp-image-78103\" title=\"-\" srcset=\"https:\/\/discover.restek.com\/wp-content\/uploads\/blog-improved-indeno-123-cd-pyrene-dibenz-ah-anthracene-separation-on-the-new-RXI-SVOCMS-column-02.png 505w, https:\/\/discover.restek.com\/wp-content\/uploads\/blog-improved-indeno-123-cd-pyrene-dibenz-ah-anthracene-separation-on-the-new-RXI-SVOCMS-column-02-223x300.png 223w\" sizes=\"auto, (max-width: 505px) 100vw, 505px\" \/><\/figure>\n\n\n\n<p><\/p>\n\n\n\n<p><em>Figure 2 &#8211; Ind\u00e9no[123-cd]pyr\u00e8ne et dibenz[ah]anthrac\u00e8ne dans un m\u00e9lange NIST SRM 1597a (extrait du GC_EV1606)<\/em><\/p>\n\n\n\n<h2 class=\"wp-block-heading\">Erreur d\u2019identification du signal ionique [276+] du dibenz[ah]anthrac\u00e8ne<\/h2>\n\n\n\n<p>Cette situation est la plus simple, mais elle peut conduire \u00e0 des r\u00e9sultats d\u00e9sastreux. Si l\u2019<strong>IcdP <\/strong>et le <strong>DahA <\/strong>co\u00e9luent pendant l\u2019analyse chromatographique, et qu\u2019un \u00e9chantillon issu d&#8217;un essai inter-laboratoire contient du <strong>DahA <\/strong>\u00e0 une concentration mod\u00e9r\u00e9ment \u00e9lev\u00e9e, il est impossible d\u2019identifier si l\u2019ion [276+] provient du <strong>DahA <\/strong>ou de l\u2019<strong>IcdP<\/strong>. Lors des essais inter-laboratoires d\u2019aptitude (EILA), des erreurs cons\u00e9cutifs dans la quantification de ces compos\u00e9s peuvent conduire l\u2019autorit\u00e9 de certification locale \u00e0 retirer la certification qui autorise le laboratoire \u00e0 effectuer ces analyses.<\/p>\n\n\n\n<h2 class=\"wp-block-heading\">Conditions analytiques recommand\u00e9es pour la colonne Rxi-SVOCms<\/h2>\n\n\n\n<p>La Figure 5 montre le niveau de contr\u00f4le CCV (Continuing Calibration Validation) (20 ng\/\u00b5l) provenant de notre \u00e9talonnage en 8 points, avec des concentrations allant de 1 ng\/\u00b5l \u00e0 120 ng\/\u00b5l, ou de 100 pg \u00e0 12 ng pour chacun des 86 compos\u00e9s cibles et des \u00e9talons de substitution sur la colonne r\u00e9f. 16623 \u2013 une colonne <strong>Rxi-SVOCms<\/strong> de 30 m x 0,25 mm x 0,25 \u00b5m (<a href=\"https:\/\/fr.restek.com\/chromatogram-detail\/GC_EV1604\" data-type=\"link\" data-id=\"https:\/\/fr.restek.com\/chromatogram-detail\/GC_EV1604\" target=\"_blank\" rel=\"noopener\">GC_EV1604<\/a>).<\/p>\n\n\n<style>.kb-image76488_dbc8c7-54 .kb-image-has-overlay:after{opacity:0.3;}<\/style>\n<figure class=\"wp-block-kadence-image kb-image76488_dbc8c7-54 size-large\"><img loading=\"lazy\" decoding=\"async\" width=\"1024\" height=\"583\" src=\"https:\/\/discover.restek.com\/wp-content\/uploads\/\/blog-improved-indeno-123-cd-pyrene-dibenz-ah-anthracene-separation-on-the-new-RXI-SVOCMS-column-03-1024x583.png\" alt=\"\" class=\"kb-img wp-image-78097\" title=\"-\" srcset=\"https:\/\/discover.restek.com\/wp-content\/uploads\/blog-improved-indeno-123-cd-pyrene-dibenz-ah-anthracene-separation-on-the-new-RXI-SVOCMS-column-03-1024x583.png 1024w, https:\/\/discover.restek.com\/wp-content\/uploads\/blog-improved-indeno-123-cd-pyrene-dibenz-ah-anthracene-separation-on-the-new-RXI-SVOCMS-column-03-300x171.png 300w, https:\/\/discover.restek.com\/wp-content\/uploads\/blog-improved-indeno-123-cd-pyrene-dibenz-ah-anthracene-separation-on-the-new-RXI-SVOCMS-column-03-768x437.png 768w, https:\/\/discover.restek.com\/wp-content\/uploads\/blog-improved-indeno-123-cd-pyrene-dibenz-ah-anthracene-separation-on-the-new-RXI-SVOCMS-column-03.png 1265w\" sizes=\"auto, (max-width: 1024px) 100vw, 1024px\" \/><\/figure>\n\n\n\n<p><\/p>\n\n\n\n<p><em>Figure 3 &#8211; GC_EV1604 &#8211; Exemple de chromatogramme TIC (courant ionique total) pour une solution \u00e9talon de 94 compos\u00e9s semi-volatils avec une injection en mode &#8220;split-10:1&#8221; de 2 ng de chaque compos\u00e9 dans la colonne<\/em><\/p>\n\n\n\n<p>La m\u00e9thode est optimis\u00e9e pour un temps d\u2019analyse de 16 minutes, ce qui permet d\u2019obtenir une excellente r\u00e9solution des deux paires de HAP critiques. Vall\u00e9e de <strong>86% <\/strong>pour le <strong>BbF <\/strong>et le <strong>BkF <\/strong>conform\u00e9ment aux valeurs rapport\u00e9es par MSD ChemStation et vall\u00e9e de<strong> 87%<\/strong> pour l\u2019<strong>IcdP <\/strong>et le <strong>DahA<\/strong>. Si ce temps d\u2019analyse (16 mins) n\u2019est pas suffisamment rapide, <a href=\"https:\/\/discover.restek.com\/gnbl5538-fr\/des-analyses-de-semi-volatils-plus-rapides-sans-sacrifier-les-separations-critiques-avec-le-logiciel-de-transfert-de-methodes-ezgc-et-une-colonne-rxi-svocms\/\" data-type=\"post\" data-id=\"76485\">rendez-vous dans un prochain article<\/a>. J\u2019y explique comment gagner 5 minutes d\u2019analyse sans impacter la s\u00e9paration des HAP critiques.<\/p>\n\n\n\n<div style=\"height:30px\" aria-hidden=\"true\" class=\"wp-block-spacer\"><\/div>\n\n\n        <div class=\"cpb\">\n            <h3 class=\"cpb-heading\">Products Mentioned<\/h3>\n            <hr class=\"cpb-heading-underline\" \/>\n            <div class=\"cpb-list\">\n                                    <div class=\"cpb-item\">\n                        <div class=\"cpb-col cpb-col--left\">\n                            <a class=\"cpb-catalog\" target=\"_blank\" rel=\"noopener noreferrer\" href=\"https:\/\/www.restek.com\/p\/16623\">                                Catalog No. 16623                            <\/a>                        <\/div>\n                        <div class=\"cpb-col cpb-col--middle\">\n                            <div class=\"cpb-title\">Colonne capillaire Rxi-SVOCms, L 30\u00a0m, DI 0.25 mm, 0.25 \u00b5m<\/div>\n                        <\/div>\n                        <div class=\"cpb-col cpb-col--right\">\n                                                            <a class=\"cpb-view-btn\" target=\"_blank\" rel=\"noopener noreferrer\" href=\"https:\/\/www.restek.com\/p\/16623\">Voir le produit<\/a>\n                                                    <\/div>\n                    <\/div>\n                            <\/div>\n        <\/div>\n        \n\n\n<div style=\"height:100px\" aria-hidden=\"true\" class=\"wp-block-spacer\"><\/div>\n\n\n\n<p><\/p>\n","protected":false},"excerpt":{"rendered":"<p>Lors du d\u00e9veloppement de la colonne Rxi-SVOCms, notre objectif \u00e9tait d\u2019optimiser la r\u00e9solution des HAP isobares tout en visant un temps de r\u00e9tention de 16 minutes pour le benzo[ghi]p\u00e9ryl\u00e8ne (BghiP) sur une colonne de 30 m x 0,25 mm x 0,25 \u00b5m en utilisant nos param\u00e8tres d\u2019acquisition des COSV en injection \u00ab split \u00bb [GC_EV1604]. La s\u00e9paration benzo[b]fluoranthene &#8211; benzo[k]fluoranthene (BbF &#8211; BkF) est la plus attractive , mais nous avons \u00e9galement  consacr\u00e9 de nombreuses ressources pour mieux s\u00e9parer  l\u2019ind\u00e9no[123-cd]pyr\u00e8ne et le dibenz[ah]anthrac\u00e8ne (IcdP &#8211; DahA) dans le temps imparti.<\/p>\n","protected":false},"author":5,"featured_media":0,"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":[791],"tags":[],"industries-application":[],"post-badge":[],"resource-type":[],"product-library":[],"resource-technique":[],"ppma_author":[584],"class_list":["post-76488","post","type-post","status-publish","format-standard","hentry","category-blog-fr"],"acf":[],"taxonomy_info":{"category":[{"value":791,"label":"Blog"}]},"featured_image_src_large":false,"author_info":{"display_name":"Brenda Cogan","author_link":"https:\/\/discover.restek.com\/fr\/author\/brenda-coganrestek-com\/"},"comment_info":0,"category_info":[{"term_id":791,"name":"Blog","slug":"blog-fr","term_group":0,"term_taxonomy_id":791,"taxonomy":"category","description":"","parent":0,"count":444,"filter":"raw","cat_ID":791,"category_count":444,"category_description":"","cat_name":"Blog","category_nicename":"blog-fr","category_parent":0}],"tag_info":false,"authors":[{"term_id":584,"user_id":0,"is_guest":1,"slug":"chris-rattray","display_name":"Chris Rattray","avatar_url":"https:\/\/secure.gravatar.com\/avatar\/?s=96&d=mm&r=g","0":null,"1":"","2":"","3":"","4":"","5":"","6":"","7":"","8":""}],"_links":{"self":[{"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/posts\/76488","targetHints":{"allow":["GET"]}}],"collection":[{"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/posts"}],"about":[{"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/types\/post"}],"author":[{"embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/users\/5"}],"replies":[{"embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/comments?post=76488"}],"version-history":[{"count":12,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/posts\/76488\/revisions"}],"predecessor-version":[{"id":85728,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/posts\/76488\/revisions\/85728"}],"wp:attachment":[{"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/media?parent=76488"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/categories?post=76488"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/tags?post=76488"},{"taxonomy":"industries-application","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/industries-application?post=76488"},{"taxonomy":"post-badge","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/post-badge?post=76488"},{"taxonomy":"resource-type","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/resource-type?post=76488"},{"taxonomy":"product-library","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/product-library?post=76488"},{"taxonomy":"resource-technique","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/resource-technique?post=76488"},{"taxonomy":"author","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/ppma_author?post=76488"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}