{"id":43577,"date":"2020-10-21T14:30:00","date_gmt":"2020-10-21T14:30:00","guid":{"rendered":"https:\/\/discover.restek.com\/uncategorized\/micotossine-nellolio-di-cbd-di-cannabis-con-la-colonna-raptor-bifenilica\/"},"modified":"2026-01-28T21:57:25","modified_gmt":"2026-01-28T21:57:25","slug":"micotossine-nellolio-di-cbd-di-cannabis-con-la-colonna-raptor-bifenilica","status":"publish","type":"post","link":"https:\/\/discover.restek.com\/it\/articoli\/ffss2946-it\/micotossine-nellolio-di-cbd-di-cannabis-con-la-colonna-raptor-bifenilica","title":{"rendered":"Analisi ad alto rendimento delle micotossine nell\u2019olio di CBD di cannabis con una semplice purificazione del campione e un\u2019eccellente sensibilit\u00e0 LC-MS\/MS"},"content":{"rendered":"\n<ul class=\"wp-block-list\">\n<li>Analizza un maggior numero di campioni per turno con un ciclo rapido della durata totale di soli 3 minuti.<\/li>\n\n\n\n<li>Rimuovi le interferenze della matrice in un unico step purificando il campione con le cartucce SPE Resprep.<\/li>\n\n\n\n<li>Ottieni un\u2019ottima sensibilit\u00e0 in matrice fino a livelli di 2 ng\/g con la strumentazione tradizionale.Fast, 3-min total cycle time lets you analyze more samples per shift.<\/li>\n<\/ul>\n\n\n\n<p>Le aflatossine e le ocratossine destano sempre pi\u00f9 preoccupazione nell\u2019industria della cannabis, poich\u00e9 questi metaboliti fungini secondari, se&nbsp;ingeriti, possono causare gravi malattie e talvolta la morte. Le colture possono subire l&#8217;attacco da parte dei funghi a partire dal seme fino allo stoccaggio, quindi le possibilit\u00e0 di contaminazione sono molteplici. Pertanto, per tutelare la salute dei consumatori e garantirne la sicurezza, emerge l\u2019esigenza di effettuare dei test per individuare la presenza di micotossine sia nelle materie prime vegetali sia nei prodotti finiti a base di cannabis. L\u2019analisi delle micotossine nell\u2019olio di cannabis \u00e8 particolarmente critica perch\u00e9 i lipidi presenti nel campione possono generare interferenze isobare della matrice, oltre a provocare una soppressione ionica che pu\u00f2 ridurre l\u2019accuratezza, soprattutto a livello di tracce.<\/p>\n\n\n\n<p>Per la preparazione del campione nelle analisi delle micotossine nella cannabis vengono comunemente impiegate le colonne di immunoaffinit\u00e0 (IAC). Tuttavia, le IAC contribuiscono in modo significativo alla complessit\u00e0 generale del metodo, ai tempi e ai costi associati a questo tipo di analisi. I metodi IAC richiedono una procedura elaborata, in quanto sono necessarie numerose fasi di condizionamento e lavaggio. Inoltre, dato che le colonne di questo tipo sono tossino-specifiche, i laboratori devono utilizzare pi\u00f9 IAC per poter analizzare tutte le micotossine di interesse.<\/p>\n\n\n\n<p>In questo studio, come alternativa alle IAC, \u00e8 stato sviluppato un semplice metodo di purificazione attraverso le cartucce SPE Resprep, applicato agli oli di CBD ad alto contenuto lipidico. Gli eccellenti risultati cromatografici ottenuti sia con le aflatossine sia con le ocratossine, persino a livelli di 2\u202fng\/g, hanno dimostrato che questa tecnica semplificata di preparazione del campione ha effettivamente rimosso le interferenze lipidiche. La purificazione del campione SPE \u00e8 stata associata a una rapida analisi LC-MS\/MS effettuata utilizzando una colonna Raptor bifenilica. Grazie alla polarizzabilit\u00e0 e alla selettivit\u00e0 unica della colonna Raptor bifenilica, tutti gli analiti target sono stati separati efficacemente con una veloce analisi della durata di soli 3\u202fminuti, confermando la superiorit\u00e0 di questo metodo rispetto alle colonne IAC per un\u2019analisi ad alto rendimento delle micotossine nell\u2019olio CBD di cannabis.<\/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 regular-image\"><img decoding=\"async\" src=\"https:\/\/ez.restek.com\/images\/cgram\/lc_gn0587.png\" alt=\"Mycotoxins in a CBD Oil Sample on Raptor Biphenyl by LC-MS\/MS\" title=\"-\"><\/div><p class=\"article-id\" style=\"text-align:center\"> LC_GN0587<\/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\">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\">Aflatoxin G2-13C17<\/td><td class=\"oth\">1.340<\/td><td class=\"oth\">348.3<\/td><td class=\"oth\">330.3<\/td><td class=\"oth\">&#8211;<\/td><\/tr>\n<tr><td class=\"num\">2.<\/td><td class=\"cmpd\">Aflatoxin G1-13C17<\/td><td class=\"oth\">1.576<\/td><td class=\"oth\">346.3<\/td><td class=\"oth\">257.3<\/td><td class=\"oth\">&#8211;<\/td><\/tr>\n<tr><td class=\"num\">3.<\/td><td class=\"cmpd\">Aflatoxin B2-13C17<\/td><td class=\"oth\">1.703<\/td><td class=\"oth\">332.3<\/td><td class=\"oth\">303.3<\/td><td class=\"oth\">&#8211;<\/td><\/tr>\n<tr><td class=\"num\">4.<\/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\">1.824<\/td><td class=\"oth\">404.3<\/td><td class=\"oth\">239.1<\/td><td class=\"oth\">358.3<\/td><\/tr>\n<tr><td class=\"num\">5.<\/td><td class=\"cmpd\">Ochratoxin A-13C20<\/td><td class=\"oth\">1.825<\/td><td class=\"oth\">424.3<\/td><td class=\"oth\">250.2<\/td><td class=\"oth\">&#8211;<\/td><\/tr>\n<tr><td class=\"num\">6.<\/td><td class=\"cmpd\">Aflatoxin B1-13C17<\/td><td class=\"oth\">1.947<\/td><td class=\"oth\">330.3<\/td><td class=\"oth\">301.4<\/td><td class=\"oth\">&#8211;<\/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 Biphenyl  (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/9309A52?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=LC_GN0587\" 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_GN0587\" rel=\"noopener\">cat.# 9309A0252<\/a>)<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Temp.:<\/th><td>35 \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>45:55 Water:Methanol<\/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><\/tr><\/thead><tbody><tr><td>0.00<\/td><td>0.7<\/td><td>35<\/td><td>65<\/td><\/tr><tr><td>2.00<\/td><td>0.7<\/td><td>10<\/td><td>90<\/td><\/tr><tr><td>2.01<\/td><td>0.7<\/td><td>35<\/td><td>65<\/td><\/tr><tr><td>3.00<\/td><td>0.7<\/td><td>35<\/td><td>65<\/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>0.25 g of commercially available hemp-derived CBD oil was weighed into a 2 mL vial. A working internal standard was prepared using 13C labeled analogs at a concentration of 250 ng\/mL in methanol. 10 \u00b5L of the working internal standard was aliquoted into the sample followed by vortexing for 10 seconds at 3000 rpm. 1 mL of 45:55 H<sub>2<\/sub>O:MeOH was added to the sample. The sample was vortexed for 30 seconds at 3000 rpm.  The sample was then centrifuged at 3000 xg for 5 min at 10 \u00b0C.  750 \u00b5L of the supernatant was transferred to a conditioned (1 mL 45:55 water:methanol) Resprep bonded reversed phase SPE cartridge (Restek cat.# 26030).  The sample was pulled through under vacuum into an autosampler vial for LC-MS\/MS 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_gn0587.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>I complessi e lunghi protocolli di preparazione del campione su colonna di immunoaffinit\u00e0 per le micotossine possono essere sostituiti da questa semplice pulizia del campione SPE pass-through. In combinazione con l&#8217;analisi LC-MS\/MS con una colonna Raptor Biphenyl, sono stati ottenuti risultati cromatografici eccellenti per le aflatossine e le ocratossine a 2 ng\/g, fornendo una soluzione ad alta produttivit\u00e0 per l&#8217;analisi delle micotossine nella cannabis.<\/p>\n","protected":false},"author":11,"featured_media":6919,"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":[2281,2243,2290,2292],"post-badge":[],"resource-type":[],"product-library":[2528,2516],"resource-technique":[2334,2337,2364],"ppma_author":[414],"class_list":["post-43577","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-articoli","industries-application-cannabis-it","industries-application-cannabis-terapeutica-ricreativa","industries-application-food-beverage-it","industries-application-sicurezza-alimentare-it","product-library-colonne-gc","product-library-prodotti-per-gascromatografia","resource-technique-cromatografia-liquida-lc","resource-technique-estrazione-in-fase-solida-spe","resource-technique-ms-ms-it"],"acf":[],"taxonomy_info":{"category":[{"value":788,"label":"Articoli"}],"industries-application":[{"value":2281,"label":"Cannabis"},{"value":2243,"label":"Cannabis Terapeutica o Ricreativa"},{"value":2290,"label":"Food &amp; 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