{"id":43576,"date":"2020-10-21T14:30:00","date_gmt":"2020-10-21T14:30:00","guid":{"rendered":"https:\/\/discover.restek.com\/uncategorized\/high-throughput-analysis-of-mycotoxins-in-cannabis-cbd-oil-pairs-simplified-cleanup-with-lc-msms-sensitivity\/"},"modified":"2026-01-28T16:57:15","modified_gmt":"2026-01-28T16:57:15","slug":"high-throughput-analysis-of-mycotoxins-in-cannabis-cbd-oil-pairs-simplified-cleanup-with-lc-msms-sensitivity","status":"publish","type":"post","link":"https:\/\/discover.restek.com\/fr\/articles\/ffss2946\/high-throughput-analysis-of-mycotoxins-in-cannabis-cbd-oil-pairs-simplified-cleanup-with-lc-msms-sensitivity","title":{"rendered":"High-Throughput Analysis of Mycotoxins in Cannabis CBD Oil Pairs Simplified Cleanup with LC-MS\/MS Sensitivity"},"content":{"rendered":"\n<ul class=\"wp-block-list\">\n<li>Fast, 3-min total cycle time lets you analyze more samples per shift.<\/li>\n\n\n\n<li>Resprep SPE sample cleanup removes matrix interferences in one simple step.<\/li>\n\n\n\n<li>Excellent sensitivity down to 2 ng\/g in matrix on legacy instrumentation.<\/li>\n<\/ul>\n\n\n\n<p>Aflatoxins and ochratoxins are an emerging concern in the cannabis industry as these secondary fungal metabolites can cause disease and death if consumed. Crops are susceptible to fungal growth from seed through storage, so there are many opportunities for contamination to occur. As a result, a growing need is emerging for testing to detect the presence of mycotoxins in both raw plant materials and finished cannabis products in order to protect consumer health and safety. The analysis of mycotoxins in cannabis oils is particularly challenging because the lipids in the sample can contribute isobaric matrix interferences in addition to general ion suppression that can reduce accuracy, particularly at low levels.<\/p>\n\n\n\n<p>Immunoaffinity columns (IACs) are commonly used for sample preparation when analyzing mycotoxins in cannabis; however, IACs also contribute significantly to the overall complexity, time, and cost associated with mycotoxin analysis. IAC methods are labor intensive, requiring numerous conditioning and washing steps. In addition, labs typically have to use multiple IACs in order to analyze all the mycotoxins of interest due to columns being specific for aflatoxins or ochratoxins.<\/p>\n\n\n\n<p>In this study, a simple pass-through SPE sample cleanup was developed as an alternative to IACs and applied to lipid-rich CBD oils. Excellent chromatographic results were obtained for both aflatoxins and ochratoxins even at 2 ng\/g, indicating that the simplified sample prep technique effectively removed lipid interferences. The SPE sample cleanup was paired with a rapid LC-MS\/MS analysis utilizing a Raptor Biphenyl column. The polarizability and unique selectivity of the Raptor Biphenyl column effectively separated all target analytes in a fast, 3-minute analysis, making this method a better approach than IACs for high-throughput testing of mycotoxins in cannabis CBD oils.<\/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:20px\" aria-hidden=\"true\" class=\"wp-block-spacer\"><\/div>\n\n\n\n<div class=\"wp-block-columns has-background is-layout-flex wp-container-core-columns-is-layout-9d6595d7 wp-block-columns-is-layout-flex\" style=\"background-color:#e4f7fa\">\n<div class=\"wp-block-column is-layout-flow wp-block-column-is-layout-flow\" style=\"flex-basis:66.66%\">\n<h3 class=\"wp-block-heading has-text-color has-link-color wp-elements-1489b0bd8c7fa6a213f7f4f1cf134d8f\" style=\"color:#02366d\">Want even better performance when analyzing mycotoxins and other metal-sensitive compounds?<\/h3>\n\n\n\n<p>Learn more at&nbsp;<a href=\"https:\/\/www.restek.com\/articles\/accurately-analyze-metal-sensitive-compounds-with-resteks-new-inert-lc-columns\" target=\"_blank\" rel=\"noopener\">www.restek.com\/inert<\/a><\/p>\n<\/div>\n\n\n\n<div class=\"wp-block-column is-layout-flow wp-block-column-is-layout-flow\" style=\"flex-basis:33.33%\">\n<figure class=\"wp-block-image size-full\"><img loading=\"lazy\" decoding=\"async\" width=\"400\" height=\"123\" src=\"https:\/\/discover.restek.com\/wp-content\/uploads\/teaser-product-lc-columns-inert-lc-02.png\" alt=\"\" class=\"wp-image-29764\" title=\"-\" srcset=\"https:\/\/discover.restek.com\/wp-content\/uploads\/teaser-product-lc-columns-inert-lc-02.png 400w, https:\/\/discover.restek.com\/wp-content\/uploads\/teaser-product-lc-columns-inert-lc-02-300x92.png 300w\" sizes=\"auto, (max-width: 400px) 100vw, 400px\" \/><\/figure>\n<\/div>\n<\/div>\n\n\n\n<div style=\"height:100px\" aria-hidden=\"true\" class=\"wp-block-spacer\"><\/div>\n","protected":false},"excerpt":{"rendered":"<p>Complex, time-consuming immunoaffinity column sample prep protocols for mycotoxins can be replaced by this simple pass-through SPE sample cleanup. Paired with LC-MS\/MS analysis using a Raptor Biphenyl column, excellent chromatographic results were obtained for aflatoxins and ochratoxins at 2 ng\/g, providing a high-throughput solution for analyzing mycotoxins in 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":[7],"tags":[],"industries-application":[2149,2167,2169,2151],"post-badge":[],"resource-type":[2623],"product-library":[2372,2384],"resource-technique":[2299,2302,2304],"ppma_author":[414],"class_list":["post-43576","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-articles","industries-application-cannabis","industries-application-food-beverage","industries-application-food-safety","industries-application-medical-or-recreational-cannabis","resource-type-featured-application","product-library-gas-chromatography-products","product-library-gc-columns","resource-technique-liquid-chromatography","resource-technique-ms-ms","resource-technique-solid-phase-extraction-spe"],"acf":[],"taxonomy_info":{"category":[{"value":7,"label":"Articles"}],"industries-application":[{"value":2149,"label":"Cannabis"},{"value":2167,"label":"Food &amp; 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