{"id":477,"date":"2023-01-10T23:21:16","date_gmt":"2023-01-10T23:21:16","guid":{"rendered":"https:\/\/graywolfslair.com\/?p=477"},"modified":"2023-03-21T22:20:47","modified_gmt":"2023-03-21T22:20:47","slug":"10-11-isolation-of-d9-thc-from-hemp-and-analytical-aspects","status":"publish","type":"post","link":"https:\/\/graywolfslair.com\/index.php\/10-the-alchemist-resource\/10-11-isolation-of-d9-thc-from-hemp-and-analytical-aspects\/","title":{"rendered":"10.11 Isolation of D9-THC from Hemp and analytical aspects"},"content":{"rendered":"\n<p><strong>Isolation of D9-THC-a from hemp and analytical aspects concerning the determination of D9-THC in cannabis products,&nbsp;<\/strong>&nbsp;<\/p>\n\n\n\n<p>by Dussy, Hamberg, Luginbiihl, Schwerzmann, and Briellmann,&nbsp;<\/p>\n\n\n\n<p>from Institute of Legal Medicine<\/p>\n\n\n\n<p>as published in Forensic Science International on line18-Aug-2004<\/p>\n\n\n\n<p>Wow, lookee what Dr Fischedick shared with me, after being kind enough to listen to my enigma.&nbsp; Still working on the puzzlement, but getting closer and had some major insights reading this study done in Switzerland by the Institute of Legal Medicine.<\/p>\n\n\n\n<p>Take a look at their extraction method at 2.2 and column chromatography purification procedure at 2.3 for lots of new ideas, and decarboxylation optimization results at 3.3, which with the Figure 8 graph, puts a whole new slant on thangs.<\/p>\n\n\n\n<p>Hee, hee, hee, enjoy and hats off to Dr Fischedick for the link!&nbsp; Copies of the study at:&nbsp;<\/p>\n\n\n\n<p><a href=\"http:\/\/www.sciencedirect.com\/science\/article\/pii\/S0379073804003408\">\u00a0http:\/\/www.sciencedirect.com\/science\/article\/pii\/S0379073804003408<\/a><\/p>\n\n\n\n<p>Here are some high points paraphrased:<\/p>\n\n\n\n<p><em>2.2. Extracting D9-THCA-a<\/em><\/p>\n\n\n\n<p><em>The extraction was done per&nbsp; Lehmann and Brenneisen&nbsp; procedure.<\/em><\/p>\n\n\n\n<p><em>100 g of 5% D9 THC content was pulverized and extracted using 500 mL petroleum ether, which hac been acidified with 0.5 mL acetic acid (0.5 mL CH3COOH in 500 mL PE).<\/em><\/p>\n\n\n\n<p><em>The filtrate was re-extracted three times, using 400 mL 2% aqueous NaOH and Na2SO3 (2% each). The 1200 mL of solution was acidified using 500 mL of 5% glacial sulfuric acid, to reach a pH of 3, followed by an immediate extraction using three times 400 mL TBME.<\/em><\/p>\n\n\n\n<p><em>The extracts were dried using Na2SO4, followed by filtration and concentration using a rotary evaporator at 25\u201330 8C. After overnight drying under vacuum, it yielded 1.71 grams of a brown amorphous solid.<\/em><\/p>\n\n\n\n<p><em>&nbsp;***<\/em><\/p>\n\n\n\n<p><em>2.3. Purifying the crude extract using column chromatography.<\/em><\/p>\n\n\n\n<p><em>They chromatographed a hundred and seventy-seven milligrams crude extract, using a&nbsp; 30 mm _ 400 mm column, packed with 0.063\u20130.2 mm 100 g silica 60 ().<\/em><\/p>\n\n\n\n<p><em>An elution solvent was used consisting of&nbsp; 650 mL hexane, 215 mL toluene, 135 mL Acetone and 20 drops of acetic acid.&nbsp; It was passed through the column at 1.5 mL\/min.&nbsp;<\/em><\/p>\n\n\n\n<p><em>D9-THCA-A began eluting at 280 mL. They collected the fractions from 290 mL until 510 mL<\/em><\/p>\n\n\n\n<p><em>and concentrated them in a 25\u201330 8C rotary evaporator at . After overnight drying under vacuum conditions it yielded 99 mg pale yellow amorphous solid.<\/em><\/p>\n\n\n\n<p><em>The sample tested 96% pure D9-THCA-A by 1H-NMR, with the principle impurity being CBN. &nbsp;<\/em><\/p>\n\n\n\n<p><em>****<\/em><\/p>\n\n\n\n<p><strong><em>Fig. 8<\/em><\/strong><em>&nbsp;shows that 150C is about the optimum THC-a decarboxylation temperature, with a yield of around 70%, the balance oxidizing into cannabinol.<\/em><\/p>\n\n\n\n<figure class=\"wp-block-image\"><img data-recalc-dims=\"1\" decoding=\"async\" src=\"https:\/\/i0.wp.com\/web.archive.org\/web\/20211026152130im_\/https%3A\/\/graywolfslair.com\/images\/Decarb_curve.jpg?w=525&#038;ssl=1\" alt=\"\"\/><\/figure>\n\n\n\n<p><strong><em>Figure 8<\/em><\/strong><\/p>\n\n\n\n<p><em>&nbsp;Given that the sum of D9-THCA-A, D9-THC and cannabinol doesn&#8217;t total 100%, the assumption is made that other polymeric material is also formed.<\/em><\/p>\n\n\n\n<p><em>A change in temperature, requires an attendant adjustment in exposure time to maximize yield.&nbsp;&nbsp;<\/em><\/p>\n\n\n\n<p><em>There is no significant temperature dependence observed between 140 and 160 C, so an exact temperature setting is not critical within that range.<\/em><\/p>\n\n\n\n<p>&nbsp;The significance that I see in graph Fig 8, is that the previous assumption has been that at 70% decarboxylation that the rate of conversion of the remaining 30% THC-a tp THC, was at a lower rate that the conversion of THC to CBN, but this graph shows THC-a to THC is maxed out at 70% and the decline in total THC is due to conversion to CBN.<\/p>\n","protected":false},"excerpt":{"rendered":"<p>Isolation of D9-THC-a from hemp and analytical aspects concerning the determination of D9-THC in cannabis products,&nbsp;&nbsp; by Dussy, Hamberg, Luginbiihl, Schwerzmann, and Briellmann,&nbsp; from Institute [&hellip;]<\/p>\n","protected":false},"author":4,"featured_media":0,"comment_status":"open","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"_jetpack_memberships_contains_paid_content":false,"footnotes":""},"categories":[45],"tags":[],"class_list":["post-477","post","type-post","status-publish","format-standard","hentry","category-10-the-alchemist-resource"],"yoast_head":"<!-- This site is optimized with the Yoast SEO plugin v27.3 - https:\/\/yoast.com\/product\/yoast-seo-wordpress\/ -->\n<title>10.11 Isolation of D9-THC from Hemp and analytical aspects - GrayWolf&#039;s Lair<\/title>\n<meta name=\"robots\" content=\"index, follow, max-snippet:-1, max-image-preview:large, max-video-preview:-1\" \/>\n<link rel=\"canonical\" href=\"https:\/\/graywolfslair.com\/index.php\/10-the-alchemist-resource\/10-11-isolation-of-d9-thc-from-hemp-and-analytical-aspects\/\" \/>\n<meta property=\"og:locale\" content=\"en_US\" \/>\n<meta property=\"og:type\" content=\"article\" \/>\n<meta property=\"og:title\" content=\"10.11 Isolation of D9-THC from Hemp and analytical aspects - GrayWolf&#039;s Lair\" \/>\n<meta property=\"og:description\" content=\"Isolation of D9-THC-a from hemp and analytical aspects concerning the determination of D9-THC in cannabis products,&nbsp;&nbsp; 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The Alchemist Resource&quot;","block_context":{"text":"10. 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