{"id":43547,"date":"2020-10-21T00:00:00","date_gmt":"2020-10-21T00:00:00","guid":{"rendered":"https:\/\/discover.restek.com\/uncategorized\/ameliorez-votre-analyse-de-lacrylamide-grace-a-une-colonne-robuste-et-un-standard-interne-certifie\/"},"modified":"2026-01-28T23:17:49","modified_gmt":"2026-01-28T23:17:49","slug":"ameliorez-votre-analyse-de-lacrylamide-grace-a-une-colonne-robuste-et-un-standard-interne-certifie","status":"publish","type":"post","link":"https:\/\/discover.restek.com\/fr\/articles-fr\/ffar3126-fr\/ameliorez-votre-analyse-de-lacrylamide-grace-a-une-colonne-robuste-et-un-standard-interne-certifie","title":{"rendered":"Am\u00e9liorez votre analyse de l\u2019acrylamide gr\u00e2ce \u00e0 une colonne robuste et un standard interne certifi\u00e9"},"content":{"rendered":"\n<p>L\u2019acrylamide peut se former dans les aliments quand des sucres r\u00e9agissent avec l\u2019acide amin\u00e9 asparagine lors de proc\u00e9d\u00e9s de cuisson \u00e0 haute temp\u00e9rature, comme la friture ou la grillade par exemple. Les aliments comme les chips, les produits \u00e0 base de c\u00e9r\u00e9ales, et le caf\u00e9 sont des exemples de produits pour lesquels on cherche \u00e0 d\u00e9terminer la pr\u00e9sence et la concentration d\u2019acrylamide.<br>La pr\u00e9sence d\u2019acrylamide dans les aliments a \u00e9t\u00e9 signal\u00e9e pour la premi\u00e8re fois par l\u2019Agence Nationale Su\u00e9doise des Aliments (Swedish National Food Administration) en 2002. Suite \u00e0 ce signalement, il y a eu partout dans le monde une augmentation constante des efforts afin de mieux comprendre son origine dans les aliments, l\u2019ampleur de la contamination dans diverses denr\u00e9es alimentaires et ses effets potentiels sur la sant\u00e9 li\u00e9s \u00e0 l\u2019exposition alimentaire. L\u2019acrylamide est class\u00e9e comme substance chimique tr\u00e8s dangereuse et il a \u00e9t\u00e9 d\u00e9montr\u00e9 qu\u2019une concentration \u00e9lev\u00e9e d\u2019acrylamide peut provoquer des cancers chez les animaux de laboratoire (m\u00eame si aucun lien direct entre l\u2019exposition alimentaire et l\u2019augmentation des cancers chez l\u2019Homme n\u2019ait \u00e9t\u00e9 prouv\u00e9 \u00e0 ce jour). Pour pr\u00e9server la Sant\u00e9 Publique, les scientifiques ont donc besoin de m\u00e9thodes d\u2019analyse qui leur permettent de d\u00e9terminer avec efficacit\u00e9 et pr\u00e9cision les concentrations d\u2019acrylamide dans les aliments et les boissons. Dans cet article, nous comparons les m\u00e9thodes d\u2019analyse typiques de l\u2019acrylamide \u00e0 une solution am\u00e9lior\u00e9e utilisant une colonne Allure Acrylamide et un standard interne deut\u00e9r\u00e9. Les b\u00e9n\u00e9fices de cette solution sont des temps d\u2019analyse plus rapides et de plus longues s\u00e9quences d\u2019analyse sans besoin d\u2019aucune maintenance instrumentale.<\/p>\n\n\n\n<h2 class=\"wp-block-heading\">Approche analytique actuelle<\/h2>\n\n\n\n<h4 class=\"wp-block-heading\">La LC-MS\/MS est la technique de choix<\/h4>\n\n\n\n<p>L\u2019analyse pr\u00e9cise de l\u2019acrylamide dans les matrices alimentaires a pr\u00e9sent\u00e9 de nombreux challenges techniques. Au d\u00e9part, la technique GC-MS\/MS \u00e9tait la technique de base car l\u2019acrylamide est une petite mol\u00e9cule, assez volatile. Cependant, cette technique reposait sur la d\u00e9rivation de l\u2019acrylamide en un compose brom\u00e9, \u00e9tape que l\u2019on pr\u00e9f\u00e9rait \u00e9viter [1]. Les m\u00e9thodes ont donc \u00e9t\u00e9 transf\u00e9r\u00e9es en LC-MS\/MS qui est alors devenue la technique de choix pour l\u2019analyse en routine de l\u2019acrylamide dans les matrices alimentaires. Les m\u00e9thodes LC-MS\/MS font tout de m\u00eame encore face \u00e0 des challenges analytiques, notamment sur la r\u00e9tention de l\u2019acrylamide et sa s\u00e9paration des compos\u00e9s interf\u00e9rents provenant de matrices complexes dans lesquelles on cherche \u00e0 l\u2019analyser.<\/p>\n\n\n\n<h4 class=\"wp-block-heading\">Utilisation de colonnes LC de Carbone Graphique Poreux (CGP)<\/h4>\n\n\n\n<p>L\u2019Europe a normalis\u00e9 une m\u00e9thode d\u2019analyse dans les aliments \u2014EN 16618:2015\u2014 qui pr\u00e9conise l\u2019utilisation d\u2019une pr\u00e9-colonne&nbsp;et d\u2019une colonne analytique en carbone graphite poreux (CGP), en partie \u00e0 cause de la difficult\u00e9 \u00e0 analyser l\u2019acrylamide en utilisant les m\u00e9canismes traditionnels de r\u00e9tention en phase inverse. Les colonnes CGP sont maintenant couramment utilis\u00e9es dans l\u2019industrie car elles retiennent suffisamment l\u2019acrylamide pour la s\u00e9parer des compos\u00e9s interf\u00e9rents provenant de la matrice qui restent pr\u00e9sents, et ce m\u00eame apr\u00e8s une proc\u00e9dure de pr\u00e9paration d\u2019\u00e9chantillons rigoureuse comme celle d\u00e9crite dans la m\u00e9thode EN. La colonne CGP est \u00e9galement capable de travailler avec des phases mobiles 100% aqueuse, des conditions dans lesquelles de nombreuses colonnes de phase inverse subiraient le ph\u00e9nom\u00e8ne d\u2019ass\u00e8chement des pores (\u201cdewetting\u201d) qui a pour cons\u00e9quence une perte de r\u00e9tention et qui n\u00e9cessite une r\u00e9g\u00e9n\u00e9ration tr\u00e8s longue de la colonne avec une phase mobile 100% organique.<\/p>\n\n\n\n<h4 class=\"wp-block-heading\">Utilisation de standards internes deut\u00e9r\u00e9s<\/h4>\n\n\n\n<p>Une quantification pr\u00e9cise est imp\u00e9rative mais la proc\u00e9dure d\u2019extraction peut induire de grandes variations la m\u00e9thode EN recommande donc l\u2019utilisation de standards internes ajout\u00e9s \u00e0 l\u2019\u00e9chantillon en m\u00eame temps que le solvant d\u2019extraction. La m\u00e9thode EN pr\u00e9conise l\u2019utilisation de standards internes deut\u00e9r\u00e9s \u00e0 la place des standards internes marqu\u00e9s au carbone couramment utilis\u00e9s pour l\u2019analyse de l\u2019acrylamide. L\u2019acrylamide-d3 est donc le standard interne de choix, et beaucoup moins on\u00e9reux que l\u2019acrylamide marqu\u00e9e au carbone.<\/p>\n\n\n\n<h4 class=\"wp-block-heading\">Exigences de la m\u00e9thode<\/h4>\n\n\n\n<p>Le temps total d\u2019analyse dans la m\u00e9thode EN 16618 : 2015 est de 8 minutes. Pour r\u00e9pondre aux exigences de la m\u00e9thode, l\u2019acrylamide ne doit pas \u00eatre \u00e9lu\u00e9e avant 1.7 minutes, mais il est n\u00e9cessaire d\u2019ajouter du temps apr\u00e8s son \u00e9lution afin de nettoyer la colonne des compos\u00e9s interf\u00e9rents provenant de la matrice encore pr\u00e9sents, m\u00eame apr\u00e8s la double extraction SPE d\u00e9crite dans la m\u00e9thode EN. Les compos\u00e9s de la matrice sont fortement retenus sur les colonnes CGP, et si elles ne sont pas suffisamment rinc\u00e9es entre chaque analyse, ces compos\u00e9s peuvent alors d\u00e9grader les performances chromatographiques au point de ne plus pouvoir atteindre les exigences de la m\u00e9thode concernant la r\u00e9tention minimale obligatoire de 1.7 minutes.<\/p>\n\n\n\n<h4 class=\"wp-block-heading\">Un retour \u00e0 la r\u00e9tention par phase inverse peut augmenter la cadence d&#8217;analyses<\/h4>\n\n\n\n<p>Lorsque les laboratoires se rapprochent du point auquel ils ne pourront plus r\u00e9pondre aux exigences de la m\u00e9thode, deux choix s\u2019offrent alors \u00e0 eux : soit proc\u00e9der \u00e0 une tr\u00e8s longue r\u00e9g\u00e9n\u00e9ration de la colonne dans l\u2019espoir de pouvoir \u00e0 nouveau r\u00e9pondre \u00e0 ces exigences, soit remplacer la pr\u00e9-colonne et \u00e9ventuellement la colonne analytique. Ces deux choix sont co\u00fbteux, et ils diminuent les cadences analytiques. Passer sur une colonne Allure Acrylamide est une meilleure alternative : sa chimie de phase inverse (brevet\u00e9e) incorpore un ligand polaire unique, qui retient l\u2019acrylamide, est compatible avec des conditions 100% aqueuses, et offre des temps d\u2019analyse plus rapides et des dur\u00e9es de vie de colonne plus longues que celles des colonnes CGP. Utiliser une pr\u00e9-colonne et une colonne Allure Acrylamide donne la possibilit\u00e9 de retenir l\u2019acrylamide assez longtemps afin de r\u00e9pondre aux exigences de la m\u00e9thode EN, sans retenir trop fortement les&nbsp; compos\u00e9s interf\u00e9rents de la matrice, ce qui permet de les \u00e9liminer rapidement de la colonne entre deux analyses. En cons\u00e9quence, les laboratoires travaillant avec les colonnes Allure Acrylamide peuvent analyser plus d\u2019\u00e9chantillons tout en utilisant moins de colonnes \u2014 une combinaison permettant des \u00e9conomies int\u00e9ressantes pour tout laboratoire. Les exemples qui suivent illustrent les b\u00e9n\u00e9fices \u00e0 utiliser une pr\u00e9-colonne et une colonne Allure Acrylamide, avec un standard interne deut\u00e9r\u00e9, pour les laboratoires \u00e0 haut d\u00e9bit d\u2019analyses.<\/p>\n\n\n\n<h4 class=\"wp-block-heading\">Temps d&#8217;analyse plus courts<\/h4>\n\n\n\n<p>Comme les compos\u00e9s de la matrice sortent rapidement de la colonne Allure Acrylamide, cette derni\u00e8re est donc capable de s\u2019\u00e9quilibrer et d\u2019\u00eatre pr\u00eate pour la prochaine injection plus rapidement qu\u2019une colonne CGP travaillant sous conditions optimales. La figure 1 montre un exemple de deux diff\u00e9rentes m\u00e9thodes, l\u2019une sur une colonne Allure Acrylamide et l\u2019autre sur une colonne de type CGP. La m\u00e9thode sur la colonne CGP a m\u00eame \u00e9t\u00e9 optimis\u00e9e \u00e0 partir de la m\u00e9thode EN, en r\u00e9duisant le temps d\u2019analyse de 8 \u00e0 7 minutes tout en gardant un temps de rin\u00e7age et de r\u00e9\u00e9quilibration optimal. Des rin\u00e7ages suppl\u00e9mentaires n\u2019am\u00e9liorent pas de fa\u00e7on significative la dur\u00e9e de vie de la colonne. L\u2019analyse de l\u2019acrylamide sur la colonne Allure Acrylamide satisfait aux exigences de la m\u00e9thode concernant la r\u00e9tention minimale de 1.7 minutes, avec une bonne s\u00e9paration des compos\u00e9s de la matrice, et avec des temps d\u2019\u00e9quilibration beaucoup plus courts. Une diminution du temps d\u2019analyse de 2.5 minutes par rapport \u00e0 la norme EN 16618:2015 et de 1.5 minutes par rapport \u00e0 la m\u00e9thode optimis\u00e9e sur la colonne CGP, permet d\u2019analyser plus d\u2019\u00e9chantillons par jour, augmentant donc la productivit\u00e9 du laboratoire.<\/p>\n\n\n<div class=\"wp-block-custom-chromatogram-article-top\"><div class=\"chromatogram-article-placeholder\"><div class=\"figure-heading\"><strong>Figure 1\u00a0<\/strong>:\u00a0Les laboratoires peuvent augmenter leur cadence d&#8217;analyse en utilisant une colonne Allure Acrylamide\u00a0car elle n\u00e9cessite des temps d&#8217;\u00e9quilibration plus courts que ceux n\u00e9cessaires \u00e0 une colonne CGP, et ce, m\u00eame avec\u00a0une matrice complexe comme les chips.<\/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 regular-image\"><img decoding=\"async\" src=\"https:\/\/ez.restek.com\/images\/cgram\/lc_fs0532.png\" alt=\"Comparison: Acrylamide Extracted from Potato Chips on an Allure Acrylamide Column vs. a Porous Graphitized Carbon Column\" title=\"-\"><\/div><p class=\"article-id\" style=\"text-align:center\"> LC_FS0532<\/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\">Conc.<br \/>(ng\/mL)<\/th><th style=\"text-align: center;width: 75px\">Precursor<\/th><th style=\"text-align: center;width: 75px\">Product<\/th><\/tr><\/thead>\n<tbody><tr><td class=\"num\">1.<\/td><td class=\"cmpd\">Acrylamide-d3 (IS)<\/td><td class=\"oth\">200<\/td><td class=\"oth\">75.1<\/td><td class=\"oth\">58.1<\/td><\/tr>\n<tr><td class=\"num\">2.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Acrylamide\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/79-06-1\/Acrylamide\" target=\"_blank\" rel=\"noopener\">Acrylamide<\/a><\/td><td class=\"oth\">Endogenous<\/td><td class=\"oth\">72.1<\/td><td class=\"oth\">55.1<\/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>See notes<\/td><\/tr><tr><td><\/td><tr><th class=\"sub conditions_header\" scope=\"row\">Temp.:<\/th><td>22 \u00b0C<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Standard\/Sample<\/th><td>Acrylamide-d3<\/td><\/tr>\n<tr><th class=\"sub conditions_header\" scope=\"row\">Diluent:<\/th><td>Water<\/td><\/tr><td><\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Inj. Vol.:<\/th><td>10 \u00b5L <\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Mobile Phase<\/th><td>A. 0.001% Formic acid in water, B. 0.001% formic acid in acetonitrile<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Flow:<\/th><td>0.4 mL\/min<\/td><\/tr><\/table><table class=\"conditions col-lg-6 col-12\"><tr><th class=\"conditions_header\" scope=\"row\">Detector<\/th><td>MS\/MS<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Ion Mode:<\/th><td>ESI+ <\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Mode:<\/th><td>MRM <\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Instrument<\/th><td>HPLC<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Sample Preparation<\/th><td>Extracted per EN 16618:2015<br \/><br \/>Weighed 2.0 g of homogenized potato chips into a 50 mL centrifuge tube. Added 40 mL water followed by the addition of internal standard. Shook by hand for 30 sec, by vortexer for 15 sec, and then on a mechanical shaker for 60 min set to maximum sample extraction agitation. Centrifuged in a refrigerated centrifuge at 10 \u00b0C, 3600 x g for 20 min. Removed the aqueous layer after centrifugation, taking care to avoid the top, fatty layer, or the solids at the bottom of the tube. Placed the aqueous extract in an appropriate container.<br \/><br \/>For cleanup, the first SPE cartridge (multimode SPE column with nonpolar, SAX, and SCX properties, 1000 mg\/6 mL) was conditioned with 3 mL methanol and x2, 6 mL aliquots of water. Passed 10 mL of the aqueous extract through the column and collected eluate. For the next cleanup step, the second SPE cartridge (crosslinked polystyrene\/poly-DVB SPE column, 500 mg\/6 mL) was conditioned with 5 mL methanol and 5 mL water. Passed the eluate from the previous step entirely through the column. Rinsed the loaded cartridge once with 4 mL water and discarded the rinsing solvent. Eluted the acrylamide with 2 mL of 60% methanol in water. Collected the sample and transferred into an evaporation tube. Placed the tube in an evaporator at a temperature no higher than 40 \u00b0C to remove the methanol. Evaporated until the final volume was 0.5\u20130.8 mL using a gentle flow of nitrogen. Transferred the final sample into an autosampler vial and analyzed by LC-MS\/MS.<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Notes<\/th><td><b>Column Details<\/b><br \/>A. <i>Allure Acrylamide column<\/i>: 5 \u03bcm, 50 mm x 2.1 mm ID analytical column (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/9167552?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=LC_FS0532\" rel=\"noopener\">cat.# 9167552<\/a>) with 5 \u03bcm, 10 mm x 2.1 mm ID guard cartridge (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/916750212?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=LC_FS0532\" rel=\"noopener\">cat.# 916750212<\/a>).<br \/>B. <i>Porous graphitized carbon column<\/i>: 5 \u03bcm, 50 mm x 2.1 mm ID analytical column with 5 \u03bcm, 10 mm x 2.1 mm ID guard cartridge.<br \/><br \/><b>Mobile Phase Gradients (%B)<\/b><br \/>A. <i>Allure Acrylamide column<\/i>: 0.00 min (0%), 1.00 min (0%), 2.00 min (90%), 2.01 min (0%), 5.50 min (0%), flow = 0.4 mL\/min.<br \/>B. <i>Porous graphitized carbon column<\/i>: 0.00 min (0%), 1.70 min (0%), 2.70 min (90%), 2.71 min (0%), 7.00 min (0%), flow = 0.4 mL\/min.<br \/><\/td><\/tr><\/table><\/div><\/div><\/div><div class=\"chromatogram-pdf-link\"><a href=\"https:\/\/ez.restek.com\/images\/cgram\/lc_fs0532.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:20px\" aria-hidden=\"true\" class=\"wp-block-spacer\"><\/div>\n\n\n\n<h4 class=\"wp-block-heading\">Dur\u00e9e de vie des colonnes sensiblement plus longue<\/h4>\n\n\n\n<p>La figure 2 illustre la grande stabilit\u00e9 du temps de r\u00e9tention de l\u2019acrylamide sur la colonne Allure Acrylamide en comparaison \u00e0 une colonne CGP, qui montre une perte de r\u00e9tention quasi-imm\u00e9diate et ne r\u00e9pond plus au crit\u00e8re de r\u00e9tention de 1.7 minutes apr\u00e8s seulement 475 injections d\u2019un \u00e9chantillon de caf\u00e9, extrait et purifi\u00e9 selon la norme EN 16618:2015. En revanche, m\u00eame apr\u00e8s 1000 injections, les performances de la colonne Allure Acrylamide restent stables et la colonne toujours pr\u00eate pour la prochaine injection. La figure 3 montre la stabilit\u00e9 du temps de r\u00e9tention de l\u2019acrylamide de la premi\u00e8re \u00e0 la milli\u00e8me injection sur la colonne Allure Acrylamide. La capacit\u00e9 de la colonne Allure Acrylamide \u00e0 \u00e9luer les compos\u00e9s interf\u00e9rents de la matrice plut\u00f4t qu\u2019\u00e0 les retenir fortement est la cl\u00e9 de la stabilit\u00e9 de ses performances sur des centaines et des centaines d\u2019injections r\u00e9p\u00e9t\u00e9es de matrice, cela sans avoir \u00e0 la r\u00e9g\u00e9n\u00e9rer ou la changer.<\/p>\n\n\n<div class=\"wp-block-custom-chromatogram-article-top\"><div class=\"chromatogram-article-placeholder\"><div class=\"figure-heading\"><strong>Figure 2\u00a0<\/strong>: La colonne Allure Acrylamide r\u00e9pond toujours aux exigences de la norme EN 16618 : 2015 m\u00eame apr\u00e8s 1 000 injections \u2014 plus de deux fois\u00a0plus d&#8217;injections que sur une colonne CGP classique..<\/div><div class='chromatogram-article-inner-full'><div class=\"chromatogram-article-inner\">\n<div class=\"wp-block-image\">\n<figure class=\"aligncenter size-large\"><img loading=\"lazy\" decoding=\"async\" width=\"1024\" height=\"629\" src=\"https:\/\/discover.restek.com\/wp-content\/uploads\/\/figure-article-FFAR3126A-UNV-02-1024x629.jpg\" alt=\"\" class=\"wp-image-19872\" title=\"-\" srcset=\"https:\/\/discover.restek.com\/wp-content\/uploads\/figure-article-FFAR3126A-UNV-02-1024x629.jpg 1024w, https:\/\/discover.restek.com\/wp-content\/uploads\/figure-article-FFAR3126A-UNV-02-300x184.jpg 300w, https:\/\/discover.restek.com\/wp-content\/uploads\/figure-article-FFAR3126A-UNV-02-768x471.jpg 768w, https:\/\/discover.restek.com\/wp-content\/uploads\/figure-article-FFAR3126A-UNV-02-1536x943.jpg 1536w, https:\/\/discover.restek.com\/wp-content\/uploads\/figure-article-FFAR3126A-UNV-02.jpg 1800w\" sizes=\"auto, (max-width: 1024px) 100vw, 1024px\" \/><\/figure>\n<\/div>\n<\/div><\/div><\/div>\n\n<div class=\"wp-block-custom-chromatogram-article-top\"><div class=\"chromatogram-article-placeholder\"><div class=\"figure-heading\"><strong>Figure 3\u00a0<\/strong>:\u00a0M\u00eame apr\u00e8s 1000 injections d\u2019un extrait de caf\u00e9, sans aucune maintenance du syst\u00e8me LC-MS\/MS\u00a0ou remplacement de la pr\u00e9-colonne, les performances de la colonne Allure Acrylamide restent inchang\u00e9es.<\/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 regular-image\"><img decoding=\"async\" src=\"https:\/\/ez.restek.com\/images\/cgram\/lc_fs0533.png\" alt=\"Lifetime Test: EN16618:2015 Coffee Extract on Allure Acrylamide (1000th Injection)\" title=\"-\"><\/div><p class=\"article-id\" style=\"text-align:center\"> LC_FS0533<\/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\">Conc.<br \/>(ng\/mL)<\/th><th style=\"text-align: center;width: 75px\">Precursor<\/th><th style=\"text-align: center;width: 75px\">Product<\/th><\/tr><\/thead>\n<tbody><tr><td class=\"num\">1.<\/td><td class=\"cmpd\">Acrylamide-d3 (IS)<\/td><td class=\"oth\">200<\/td><td class=\"oth\">75.1<\/td><td class=\"oth\">58.1<\/td><\/tr>\n<tr><td class=\"num\">2.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Acrylamide\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/79-06-1\/Acrylamide\" target=\"_blank\" rel=\"noopener\">Acrylamide<\/a><\/td><td class=\"oth\">Endogenous<\/td><td class=\"oth\">72.1<\/td><td class=\"oth\">55.1<\/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>Allure Acrylamide  (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/9167552?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=LC_FS0533\" rel=\"noopener\">cat.# 9167552<\/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>5 \u00b5m<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Pore Size:<\/th><td>60 \u00c5<\/td><\/tr><tr><td><\/td><tr><th class=\"sub conditions_header\" scope=\"row\">Guard Column:<\/th><td>Allure Acrylamide 10 mm, 2.1 mm ID, 5 \u00b5m (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/916750212?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=LC_FS0533\" rel=\"noopener\">cat.# 916750212<\/a>)<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Temp.:<\/th><td>22 \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>Water<\/td><\/tr><td><\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Inj. Vol.:<\/th><td>10 \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>0.001% Formic acid in water <\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">B:<\/th><td>0.001% 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>0.4<\/td><td>100<\/td><td>0<\/td><\/tr><tr><td>1.00<\/td><td>0.4<\/td><td>100<\/td><td>0<\/td><\/tr><tr><td>2.00<\/td><td>0.4<\/td><td>10<\/td><td>90<\/td><\/tr><tr><td>2.01<\/td><td>0.4<\/td><td>100<\/td><td>0<\/td><\/tr><tr><td>5.50<\/td><td>0.4<\/td><td>100<\/td><td>0<\/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><th class=\"sub conditions_header\" scope=\"row\">Mode:<\/th><td>MRM <\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Instrument<\/th><td>HPLC<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Sample Preparation<\/th><td>Extracted per EN 16618:2015<br \/><br \/>Weighed 2.0 g of ground coffee into a 50 mL centrifuge tube. Added 5 mL <i>n<\/i>-hexane and 40 mL water followed by the addition of internal standard. Shook by hand for 30 sec, by vortexer for 15 sec, and then on a mechanical shaker for 60 min set to maximum sample extraction agitation. Centrifuged in a refrigerated centrifuge at 10 \u00b0C, 3600 x g for 20 min. Removed the aqueous layer after centrifugation, taking care to avoid the top, hexane layer, or the solids at the bottom of the tube. Placed the aqueous extract in an appropriate container.<br \/><br \/>For cleanup, the first SPE cartridge (multimode SPE column with nonpolar, SAX and SCX properties, 1000 mg\/6 mL) was conditioned with 3 mL methanol and x2, 6 mL aliquots of water. Passed 10 mL of the aqueous extract through the column and collected eluate. For the next cleanup step, the second SPE cartridge (crosslinked polystyrene\/poly-DVB SPE column, 500 mg\/6 mL) was conditioned with 5 mL methanol and 5 mL water. Passed the eluate from the previous step entirely through the column. Rinsed the loaded cartridge once with 4 mL water and discarded the rinsing solvent. Eluted the acrylamide with 2 mL of 60% methanol in water. Collected the sample and transferred into an evaporation tube. Placed the tube in an evaporator at a temperature no higher than 40 \u00b0C to remove the methanol. Evaporated until the final volume was 0.5\u20130.8 mL using a gentle flow of nitrogen. Transferred the final sample into an autosampler vial and analyzed by LC-MS\/MS.<\/td><\/tr><\/table><\/div><\/div><\/div><div class=\"chromatogram-pdf-link\"><a href=\"https:\/\/ez.restek.com\/images\/cgram\/lc_fs0533.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:20px\" aria-hidden=\"true\" class=\"wp-block-spacer\"><\/div>\n\n\n\n<h4 class=\"wp-block-heading\">Une meilleure solution pour l&#8217;analyse de l&#8217;acrylamide<\/h4>\n\n\n\n<p>Bien que les colonnes CGP pr\u00e9conis\u00e9es par la norme EN 16618:2015 retiennent suffisamment l\u2019acrylamide, leur forte r\u00e9tention des compos\u00e9s provenant de la matrice a pour cons\u00e9quences des temps d\u2019\u00e9quilibration plus longs et des dur\u00e9es de vie de colonne plus faibles. L\u2019analyse de l\u2019acrylamide sera plus rapide gr\u00e2ce aux colonnes Allure Acrylamide car elles garantissent une r\u00e9tention suffisante de ce compos\u00e9 tout en \u00e9liminant plus efficacement les compos\u00e9s de la matrice. En cons\u00e9quence, les exigences li\u00e9es \u00e0 la m\u00e9thode sont maintenues sur plus d\u2019injections, ce qui permet d\u2019analyser plus d\u2019\u00e9chantillons avant qu\u2019une quelconque maintenance ne soit n\u00e9cessaire. En associant les pr\u00e9-colonne et colonne analytique Allure Acrylamide \u00e0 un standard interne deut\u00e9r\u00e9, les laboratoires peuvent alors augmenter leur productivit\u00e9 et leur rentabilit\u00e9.<\/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>J.A.G. Roach, D. Andrzejewski, M.L. Gay, D. Nortrup, S.M. Musser, Rugged LC-MS\/MS survey analysis for acrylamide in foods, J. Agric. Food Chem. 51 (2003) 7547\u22127554.\u00a0<a href=\"https:\/\/pubs.acs.org\/doi\/abs\/10.1021\/jf0346354\" target=\"_blank\" rel=\"noopener\">https:\/\/pubs.acs.org\/doi\/abs\/10.1021\/jf0346354<\/a><\/li>\n<\/ol>\n\n\n\n<div style=\"height:100px\" aria-hidden=\"true\" class=\"wp-block-spacer\"><\/div>\n","protected":false},"excerpt":{"rendered":"<p>Id\u00e9ale pour augmenter le d\u00e9bit d&#8217;\u00e9chantillons, en conformit\u00e9 avec la norme EN 16618:2015, la nouvelle colonne LC Allure Acrylamide offre des temps d\u2019analyse plus rapides et des dur\u00e9es de vie de colonne plus longues que celles des colonnes de Carbone Graphite Poreux.<\/p>\n","protected":false},"author":11,"featured_media":70533,"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":[2463,2446,2471,2445],"resource-technique":[2318,2321,2362],"ppma_author":[414],"class_list":["post-43547","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-etalons-de-reference","product-library-etalons-en-solution","product-library-produits-pour-la-chromatographie-en-phase-liquide","resource-technique-chromatographie-en-phase-liquide","resource-technique-extraction-en-phase-solide-spe","resource-technique-ms-ms-fr"],"acf":[],"taxonomy_info":{"category":[{"value":462,"label":"Articles"}],"industries-application":[{"value":2214,"label":"Industrie Agroalimentaire"},{"value":2216,"label":"S\u00e9curit\u00e9 alimentaire"}],"product-library":[{"value":2463,"label":"Colonnes LC"},{"value":2446,"label":"\u00c9talons de R\u00e9f\u00e9rence"},{"value":2471,"label":"\u00c9talons en solution"},{"value":2445,"label":"Produits pour la chromatographie en phase liquide"}],"resource-technique":[{"value":2318,"label":"Chromatographie en phase liquide"},{"value":2321,"label":"Extraction en phase solide (SPE)"},{"value":2362,"label":"MS\/MS"}]},"featured_image_src_large":["https:\/\/discover.restek.com\/wp-content\/uploads\/feature-FFAR3126-1024x536.jpg",1024,536,true],"author_info":{"display_name":"Restek Corporation","author_link":"https:\/\/discover.restek.com\/fr\/author\/restek-corporation\/"},"comment_info":0,"category_info":[{"term_id":462,"name":"Articles","slug":"articles-fr","term_group":0,"term_taxonomy_id":462,"taxonomy":"category","description":"","parent":0,"count":465,"filter":"raw","cat_ID":462,"category_count":465,"category_description":"","cat_name":"Articles","category_nicename":"articles-fr","category_parent":0}],"tag_info":false,"authors":[{"term_id":414,"user_id":11,"is_guest":0,"slug":"restek-corporation","display_name":"Restek Corporation","avatar_url":{"url":"https:\/\/discover.restek.com\/wp-content\/uploads\/Restek_Favicon_300x300.jpg","url2x":"https:\/\/discover.restek.com\/wp-content\/uploads\/Restek_Favicon_300x300.jpg"},"0":null,"1":"","2":"","3":"","4":"","5":"","6":"","7":"","8":""}],"_links":{"self":[{"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/posts\/43547","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\/11"}],"replies":[{"embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/comments?post=43547"}],"version-history":[{"count":8,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/posts\/43547\/revisions"}],"predecessor-version":[{"id":85816,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/posts\/43547\/revisions\/85816"}],"wp:featuredmedia":[{"embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/media\/70533"}],"wp:attachment":[{"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/media?parent=43547"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/categories?post=43547"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/tags?post=43547"},{"taxonomy":"industries-application","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/industries-application?post=43547"},{"taxonomy":"post-badge","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/post-badge?post=43547"},{"taxonomy":"resource-type","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/resource-type?post=43547"},{"taxonomy":"product-library","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/product-library?post=43547"},{"taxonomy":"resource-technique","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/resource-technique?post=43547"},{"taxonomy":"author","embeddable":true,"href":"https:\/\/discover.restek.com\/fr\/wp-json\/wp\/v2\/ppma_author?post=43547"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}