{"id":43581,"date":"2020-10-21T14:30:00","date_gmt":"2020-10-21T14:30:00","guid":{"rendered":"https:\/\/discover.restek.com\/uncategorized\/analisi-lc-msms-delle-micotossine-nella-polvere-di-arachidi-in-55-minuti\/"},"modified":"2026-02-19T20:41:59","modified_gmt":"2026-02-19T20:41:59","slug":"analisi-lc-msms-delle-micotossine-nella-polvere-di-arachidi-in-55-minuti","status":"publish","type":"post","link":"https:\/\/discover.restek.com\/it\/articoli\/ffss2971-it\/analisi-lc-msms-delle-micotossine-nella-polvere-di-arachidi-in-55-minuti","title":{"rendered":"Analisi LC-MS\/MS delle micotossine nella polvere di arachidi in 5,5 minuti"},"content":{"rendered":"\n<ul class=\"wp-block-list\">\n<li>Analisi veloce per una maggiore produttivit\u00e0 del campione<\/li>\n\n\n\n<li>Una separazione eccellente migliora l&#8217;accuratezza per 12 micotossine regolamentate.<\/li>\n\n\n\n<li>Preparazione del campione facile e veloce (diluire-filtrare-iniettare)<\/li>\n<\/ul>\n\n\n\n<p>Alcuni funghi che crescono sui prodotti agricoli producono metaboliti tossici noti come micotossine. I moderni processi di lavorazione degli alimenti non sono in grado di rimuovere completamente questi composti, se presenti; pertanto, sono stati stabiliti rigidi protocolli di monitoraggio. Sebbene un metodo universale per l&#8217;analisi delle micotossine permetterebbe uno screening altamente efficiente, \u00e8 molto difficile svilupparne uno a causa di differenze nelle propriet\u00e0 fisico-chimiche delle micotossine, nell&#8217;efficienza di estrazione e negli effetti matrice. Zhang et al. hanno pubblicato uno studio realizzato in diversi laboratori [1] volto a fornire ai laboratori una procedura analitica che potrebbe essere ampiamente applicata all&#8217;analisi di un\u2019ampia variet\u00e0 di micotossine in diverse matrici. Ispirandoci a questo lavoro, abbiamo sviluppato il seguente metodo LC-MS\/MS che risolve 12 micotossine regolamentate dalla FDA entro i limiti di pressione degli strumenti HPLC tradizionali.<\/p>\n\n\n\n<p>In questo esempio, le micotossine sono state analizzate in una matrice di polvere di arachidi. L&#8217;uso di una colonna relativamente corta, la selettivit\u00e0 della fase stazionaria Bifenile e l&#8217;efficienza di particelle Raptor con superficie porosa da 2,7 \u00b5m hanno consentito un&#8217;eccellente e rapida separazione in 5,5 minuti (tempo ciclo totale 7 minuti). \u00c8 stato osservato un composto coeluente della matrice che condivideva la pi\u00f9 abbondante transizione MRM per la micotossina HT-2 (447,3-285,3), quindi \u00e8 stata selezionata una transizione meno abbondante (447,3-345,3) per la quantificazione. Per aumentare la sensibilit\u00e0, \u00e8 stato usato un tampone ammonio per agevolare la ionizzazione delle micotossine. La colonna Raptor Bifenile funzionava molto bene per le 12 micotossine analizzate nello studio citato, ma per gli elenchi di composti pi\u00f9 lunghi contenenti micotossine isobariche con strutture simili, la fase Raptor Fluorofenile pu\u00f2 essere necessaria per fornire un&#8217;adeguata risoluzione cromatografica. La selettivit\u00e0 della colonna Raptor Fluorofenile \u00e8 dimostrata in&nbsp;<a href=\"https:\/\/discover.restek.com\/articles\/ffss2790\/highly-selective-lc-msms-analysis-of-mycotoxins-from-multiple-classes\" data-type=\"post\" data-id=\"43565\">questa analisi di 20 micotossine<\/a>.<\/p>\n\n\n\n<p>Questo metodo ha mostrato un&#8217;eccellente precisione e accuratezza per le 12 micotossine regolamentate dalla FDA che sono state valutate durante uno studio di convalida che copriva una grande variet\u00e0 di matrici (comprese farine di mais e di riso integrale di varie origini, oltre alla polvere di arachidi qui mostrata). Restek desidera ringraziare il Dott. Zhang per il suo supporto tecnico nel corso del presente progetto.<\/p>\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_fs0526.png\" alt=\"Mycotoxins in Peanut Powder on Raptor Biphenyl by LC-MS\/MS\" title=\"-\"><\/div><p class=\"article-id\" style=\"text-align:center\"> LC_FS0526<\/p><div class=\"chromatogram-peaks\"><h4>Peaks<\/h4><table class=\"peaks col-lg-6 col-12 peak-50\">\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\/g)<\/th><th style=\"text-align: center;width: 75px\">Precursor Ion<\/th><th style=\"text-align: center;width: 75px\">Product Ion 1<\/th><th style=\"text-align: center;width: 75px\">Product Ion 2<\/th><\/tr><\/thead>\n<tbody><tr><td class=\"num\">1.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Deoxynivalenol\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/51481-10-8\/Deoxynivalenol\" target=\"_blank\" rel=\"noopener\">Deoxynivalenol<\/a><\/td><td class=\"oth\">0.62<\/td><td class=\"oth\">50<\/td><td class=\"oth\">297.3<\/td><td class=\"oth\">249.3<\/td><td class=\"oth\">231.2<\/td><\/tr>\n<tr><td class=\"num\">2.<\/td><td class=\"cmpd\">Fumonisin B1<\/td><td class=\"oth\">2.45<\/td><td class=\"oth\">50<\/td><td class=\"oth\">722.5<\/td><td class=\"oth\">352.4<\/td><td class=\"oth\">334.5<\/td><\/tr>\n<tr><td class=\"num\">3.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for HT-2\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/26934-87-2\/HT-2\" target=\"_blank\" rel=\"noopener\">HT-2<\/a><\/td><td class=\"oth\">2.60<\/td><td class=\"oth\">50<\/td><td class=\"oth\">447.3<\/td><td class=\"oth\">345.3<\/td><td class=\"oth\">285.3<\/td><\/tr>\n<tr><td class=\"num\">4.<\/td><td class=\"cmpd\">Fumonisin B3<\/td><td class=\"oth\">2.85<\/td><td class=\"oth\">50<\/td><td class=\"oth\">706.5<\/td><td class=\"oth\">336.4<\/td><td class=\"oth\">318.4<\/td><\/tr>\n<tr><td class=\"num\">5.<\/td><td class=\"cmpd\">Fumonisin B2<\/td><td class=\"oth\">3.23<\/td><td class=\"oth\">50<\/td><td class=\"oth\">706.5<\/td><td class=\"oth\">336.3<\/td><td class=\"oth\">141.2<\/td><\/tr>\n<tr><td class=\"num\">6.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for T2\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/50-31-7\/T2\" target=\"_blank\" rel=\"noopener\">T2<\/a><\/td><td class=\"oth\">3.31<\/td><td class=\"oth\">50<\/td><td class=\"oth\">489.3<\/td><td class=\"oth\">245.2<\/td><td class=\"oth\">387.4<\/td><\/tr>\n<\/tbody><\/table>\n<table class=\"peaks col-lg-6 col-12 peak-50\"><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\/g)<\/th><th style=\"text-align: center;width: 75px\">Precursor Ion<\/th><th style=\"text-align: center;width: 75px\">Product Ion 1<\/th><th style=\"text-align: center;width: 75px\">Product Ion 2<\/th><\/tr><\/thead><tbody>\n<tr><td class=\"num\">7.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Aflatoxin G2\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/7241-98-7\/Aflatoxin G2\" target=\"_blank\" rel=\"noopener\">Aflatoxin G2<\/a><\/td><td class=\"oth\">3.74<\/td><td class=\"oth\">5<\/td><td class=\"oth\">331.2<\/td><td class=\"oth\">313.3<\/td><td class=\"oth\">189.3<\/td><\/tr>\n<tr><td class=\"num\">8.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Zearalenone\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/17924-92-4\/Zearalenone\" target=\"_blank\" rel=\"noopener\">Zearalenone<\/a><\/td><td class=\"oth\">3.96<\/td><td class=\"oth\">50<\/td><td class=\"oth\">319.3<\/td><td class=\"oth\">283.3<\/td><td class=\"oth\">187.2<\/td><\/tr>\n<tr><td class=\"num\">9.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Aflatoxin G1\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/1165-39-5\/Aflatoxin G1\" target=\"_blank\" rel=\"noopener\">Aflatoxin G1<\/a><\/td><td class=\"oth\">4.22<\/td><td class=\"oth\">5<\/td><td class=\"oth\">329.2<\/td><td class=\"oth\">243.2<\/td><td class=\"oth\">200.2<\/td><\/tr>\n<tr><td class=\"num\">10.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Aflatoxin B2\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/7220-81-7\/Aflatoxin B2\" target=\"_blank\" rel=\"noopener\">Aflatoxin B2<\/a><\/td><td class=\"oth\">4.43<\/td><td class=\"oth\">5<\/td><td class=\"oth\">315.3<\/td><td class=\"oth\">287.3<\/td><td class=\"oth\">259.2<\/td><\/tr>\n<tr><td class=\"num\">11.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Aflatoxin B1\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/1162-65-8\/Aflatoxin B1\" target=\"_blank\" rel=\"noopener\">Aflatoxin B1<\/a><\/td><td class=\"oth\">4.99<\/td><td class=\"oth\">5<\/td><td class=\"oth\">313.3<\/td><td class=\"oth\">285.2<\/td><td class=\"oth\">241.2<\/td><\/tr>\n<tr><td class=\"num\">12.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Ochratoxin A\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/303-47-9\/Ochratoxin A\" target=\"_blank\" rel=\"noopener\">Ochratoxin A<\/a><\/td><td class=\"oth\">5.19<\/td><td class=\"oth\">5<\/td><td class=\"oth\">404.2<\/td><td class=\"oth\">239.3<\/td><td class=\"oth\">358.3<\/td><\/tr>\n<\/tbody><\/table><div class=\"peaknotes\">Matrix interference was observed for HT-2 transition 447.3-285.3 in peanut powder. Therefore, 447.3-345.3 was chose for quantification.<\/div><\/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 Biphenyl  (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/9309A52?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=LC_FS0526\" rel=\"noopener\">cat.# 9309A52<\/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\">Guard Column:<\/th><td>Raptor Biphenyl EXP guard column cartridge 5 mm, 2.1 mm ID, 2.7 \u00b5m (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/9309A0252?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=LC_FS0526\" rel=\"noopener\">cat.# 9309A0252<\/a>)<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Temp.:<\/th><td>40 \u00b0C<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Standard\/Sample<\/th><td><\/td><\/tr><td><\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Inj. Vol.:<\/th><td>5 \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>Water, 2 mM ammonium formate, 0.1% formic acid <\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">B:<\/th><td>Methanol, 2 mM ammonium formate, 0.1% formic acid <\/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><th>%C<\/th><\/tr><\/thead><tbody><tr><td>0.00<\/td><td>0.5<\/td><td>70<\/td><td>30<\/td><td><\/td><\/tr><tr><td>0.6<\/td><td>0.5<\/td><td>70<\/td><td>30<\/td><td><\/td><\/tr><tr><td>0.7<\/td><td>0.5<\/td><td>50<\/td><td>50<\/td><td><\/td><\/tr><tr><td>3.0<\/td><td>0.5<\/td><td>25<\/td><td>70<\/td><td><\/td><\/tr><tr><td>4.5<\/td><td>0.5<\/td><td>25<\/td><td>75<\/td><td><\/td><\/tr><tr><td>5.0<\/td><td>0.5<\/td><td>10<\/td><td>90<\/td><td><\/td><\/tr><tr><td>5.2<\/td><td>0.5<\/td><td>10<\/td><td>90<\/td><td><\/td><\/tr><tr><td>5.21<\/td><td>0.5<\/td><td>25<\/td><td>75<\/td><td><\/td><\/tr><tr><td>6.00<\/td><td>0.5<\/td><td>25<\/td><td>75<\/td><td><\/td><\/tr><tr><td>6.01<\/td><td>0.5<\/td><td>70<\/td><td>30<\/td><td><\/td><\/tr><tr><td>7.00<\/td><td>0.5<\/td><td>70<\/td><td>30<\/td><td> <\/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>UHPLC<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Sample Preparation<\/th><td>Weighed 1.00 gram of peanut powder in a 50 mL centrifuge tube and added 2.00 mL of water. Vortexed at 3000 rpm for 5 min followed by the addition of 4.0 mL of extraction solvent (50:50 water:acetonitrile, v\/v). The tube was then vortexed at 3000 rpm for 5 min followed by centrifugation for 15 min at 4200 rpm. 475 \u03bcL of the supernatant was filtered through a Thomson SINGLE StEP Nano filter vial (0.2 \u03bcm). The sample was then fortified with 25 \u03bcL of a standard solution prepared in water at 1000 ng\/mL (100 ng\/mL for aflatoxins and ochratoxin A) as part of the matrix-matched calibration curve. Vortexed at 3000 rpm for 1 min prior to analysis.<\/td><\/tr><tr class=\"cgram_header_row\"><th class=\"conditions_header\" scope=\"row\">Notes<\/th><td>Want even better performance when analyzing metal-sensitive compounds? Check out Inert LC columns at <a href=\"https:\/\/www.restek.com\/inert\" target=\"_blank\" rel=\"noopener\">www.restek.com\/inert<\/a>. <\/td><\/tr><\/table><\/div><\/div><\/div><div class=\"chromatogram-pdf-link\"><a href=\"https:\/\/ez.restek.com\/images\/cgram\/lc_fs0526.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<h2 class=\"wp-block-heading\"><strong>Riferimenti<\/strong><\/h2>\n\n\n\n<ol class=\"wp-block-list\">\n<li>K. Zhang, M.R. Schaab, G. Southwood, E.R. Tor, L.S. Aston, W. Song, B. Eitzer, S. Majumdar, T. Lapainis, H. Mai, K. Tran, A. El-Demerdash, V. Vega, Y. Cai, J.W. Wong, A.J. Krynitsky, T.H. Begley, A collaborative study: determination of mycotoxins in corn, peanut butter, and wheat flour using stable isotope dilution assay (SIDA) and liquid chromatography-tandem mass spectrometry (LC-MS\/MS), Journal of Agricultural and Food Chemistry, 65 (33) (2017) 7138-7152.&nbsp;<a href=\"https:\/\/www.ncbi.nlm.nih.gov\/pubmed\/27983809\" target=\"_blank\" rel=\"noopener\">https:\/\/www.ncbi.nlm.nih.gov\/pubmed\/27983809<\/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>Il metodo qui sviluppato fornisce un&#8217;analisi veloce delle micotossine nella polvere di arachidi. La separazione di base di 12 micotossine regolamentate dalla FDA e dall&#8217;UE \u00e8 stata ottenuta in un&#8217;analisi di 5,5 minuti (7 minuti di tempo di ciclo totale). Questo metodo pu\u00f2 essere applicato a diverse matrici utilizzando una calibrazione abbinata alla matrice o un test di diluizione con isotopi stabili. La produzione di campioni pu\u00f2 essere notevolmente aumentata grazie al breve tempo di ciclo per ogni analisi.<\/p>\n","protected":false},"author":11,"featured_media":6925,"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":[788],"tags":[],"industries-application":[2290,2292],"post-badge":[],"resource-type":[2768],"product-library":[2535,2517,2519,2549],"resource-technique":[2334,2364],"ppma_author":[414],"class_list":["post-43581","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-articoli","industries-application-food-beverage-it","industries-application-sicurezza-alimentare-it","resource-type-featured-application","product-library-colonne-lc","product-library-prodotti-per-cromatografia-liquida","product-library-prodotti-per-la-preparazione-del-campione","product-library-vial-accessori","resource-technique-cromatografia-liquida-lc","resource-technique-ms-ms-it"],"acf":[],"taxonomy_info":{"category":[{"value":788,"label":"Articoli"}],"industries-application":[{"value":2290,"label":"Food &amp; 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