{"id":43603,"date":"2021-01-12T00:00:00","date_gmt":"2021-01-12T00:00:00","guid":{"rendered":"https:\/\/discover.restek.com\/uncategorized\/fast-and-rugged-direct-analysis-of-polar-pesticides-in-spinach\/"},"modified":"2026-01-28T16:53:11","modified_gmt":"2026-01-28T16:53:11","slug":"fast-and-rugged-direct-analysis-of-polar-pesticides-in-spinach","status":"publish","type":"post","link":"https:\/\/discover.restek.com\/es\/articles\/fsfa3215\/fast-and-rugged-direct-analysis-of-polar-pesticides-in-spinach","title":{"rendered":"Fast and Rugged Direct Analysis of Polar Pesticides in Spinach"},"content":{"rendered":"\n<ul class=\"wp-block-list\">\n<li>No time-consuming derivatization, ion-pairing steps, or long waits for column equilibration.<\/li>\n\n\n\n<li>Unique stationary phase provides good retention and efficient elution, resulting in better peak shape.<\/li>\n\n\n\n<li>Robust column performance ensures consistent chromatography and reliable results.<\/li>\n<\/ul>\n\n\n\n<p>The direct analysis of polar pesticides, such as glyphosate, its main metabolite AMPA, and glufosinate, is difficult because they are not retained well on reversed phase columns, and chelation with metal surfaces in the LC-MS\/MS can significantly reduce response. Derivatization and ion-pairing reagents are often used to improve performance, but they require additional sample preparation time and can produce unfavorable side effects (precipitates, long equilibration times, system contamination, etc.).<\/p>\n\n\n\n<p>Using a Raptor Polar X column is a better solution because the novel stationary phase offers stronger interaction with polar anionic compounds. It features hybrid retention modes (HILIC and ion exchange) and provides strong retention yet allows analytes to be quickly eluted as symmetrical peaks through simple mobile phase changes. In this analysis of polar pesticides in spinach, excellent chromatographic performance is seen for all three compounds with a total analysis time of just eight minutes. Further, peak shapes and retention times remain stable over hundreds of matrix injections, and a simple guard column change restores full performance. This fast, simple, and effective workflow is a good alternative for food labs interested in the direct analysis of polar pesticides without the need for complex and time-consuming procedures.<\/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_fs0547.png\" alt=\"Polar Pesticides in Spinach on Raptor Polar X by LC-MS\/MS\" title=\"-\"><\/div><p class=\"article-id\" style=\"text-align:center\"> LC_FS0547<\/p><div class=\"chromatogram-peaks\"><h4>Peaks<\/h4><table class=\"peaks 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 Ion<\/th><th style=\"text-align: center;width: 75px\">Product Ion 1<\/th><th style=\"text-align: center;width: 75px\">Product Ion 2<\/th><th style=\"text-align: center;width: 75px\">Product Ion 3<\/th><\/tr><\/thead>\n<tbody><tr><td class=\"num\">1.<\/td><td class=\"cmpd\">AMPA<\/td><td class=\"oth\">100<\/td><td class=\"oth\">110.10<\/td><td class=\"oth\">79.05<\/td><td class=\"oth\">63.10<\/td><td class=\"oth\">81.10<\/td><\/tr>\n<tr><td class=\"num\">2.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Glufosinate\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/51276-47-2\/Glufosinate\" target=\"_blank\" rel=\"noopener\">Glufosinate<\/a><\/td><td class=\"oth\">100<\/td><td class=\"oth\">180.20<\/td><td class=\"oth\">85.15<\/td><td class=\"oth\">95.10<\/td><td class=\"oth\">&#8211;<\/td><\/tr>\n<tr><td class=\"num\">3.<\/td><td class=\"cmpd\"><a class=\"cmpd_link\" title=\"View compound information for Glyphosate\" href=\"https:\/\/ez.restek.com\/compound\/view\/en\/1071-83-6\/Glyphosate\" target=\"_blank\" rel=\"noopener\">Glyphosate<\/a><\/td><td class=\"oth\">100<\/td><td class=\"oth\">168.10<\/td><td class=\"oth\">63.05<\/td><td class=\"oth\">79.05<\/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 Polar X  (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/9311A32?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=LC_FS0547\" rel=\"noopener\">cat.# 9311A32<\/a>)<\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Dimensions:<\/th><td>30 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 Polar X guard column cartridge 5 mm, 2.1 mm ID, 2.7 \u00b5m (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/9311A0252?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=LC_FS0547\" rel=\"noopener\">cat.# 9311A0252<\/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>Spinach extract<\/td><\/tr>\n<td><\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">Inj. Vol.:<\/th><td>2 \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,  0.5% formic acid <\/td><\/tr><tr><th class=\"sub conditions_header\" scope=\"row\">B:<\/th><td>Acetonitrile, 0.5% 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>0.5<\/td><td>35<\/td><td>65<\/td><\/tr><tr><td>5.0<\/td><td>0.5<\/td><td>90<\/td><td>10<\/td><\/tr><tr><td>6.5<\/td><td>0.5<\/td><td>90<\/td><td>10<\/td><\/tr><tr><td>6.51<\/td><td>0.5<\/td><td>35<\/td><td>65<\/td><\/tr><tr><td>8<\/td><td>0.5<\/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>Frozen spinach was added to a Blixer processor with dry ice (3:1-4:1 ratio) and then ground into a very fine powder. The homogenate was placed into the freezer immediately. A 5.0 gram sample of the spinach powder was weighed into a 50 mL centrifuge tube (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/25846?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=LC_FS0547\" rel=\"noopener\">cat.# 25846<\/a>). According to the QuPPe method (Quick Polar Pesticides Method), 5.0 mL of methanol with 1.0% formic acid was added into the centrifuge tube. The tube was shaken by hand for 1 min and then by a mechanical shaker vigorously for 5 min. After centrifuging for 10 min at 4200 rpm, the supernatant was filtered through a 0.22 \u03bcm filter (<a target=\"_blank\" href=\"https:\/\/www.restek.com\/p\/23984?utm_source=chromatograms&amp;utm_medium=link&amp;utm_campaign=LC_FS0547\" rel=\"noopener\">cat.# 23984<\/a>). The final extract was fortified with the AMPA, glufosinate, and glyphosate at a final concentration of 100 ng\/mL.<\/td><\/tr><\/table><\/div><\/div><\/div><div class=\"chromatogram-pdf-link\"><a href=\"https:\/\/ez.restek.com\/images\/cgram\/lc_fs0547.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>This fast, simple LC-MS\/MS workflow for the direct analysis of polar pesticides in spinach provides good retention and peak shape over hundreds of matrix injections on a Raptor Polar X column.<\/p>\n","protected":false},"author":11,"featured_media":70560,"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":[2167,2169],"post-badge":[],"resource-type":[2623],"product-library":[2391,2373],"resource-technique":[2299,2302],"hf_cat_post":[650,2624],"ppma_author":[414],"class_list":["post-43603","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-articles","industries-application-food-beverage","industries-application-food-safety","resource-type-featured-application","product-library-lc-columns","product-library-liquid-chromatography-products","resource-technique-liquid-chromatography","resource-technique-ms-ms"],"acf":[],"taxonomy_info":{"category":[{"value":7,"label":"Articles"}],"industries-application":[{"value":2167,"label":"Food &amp; 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