Gallo-Molina Ada C, Sánchez-Correa César A, Gil-Chaves Iván D
Grupo de Procesos Químicos y Bioquímicos, Department of Chemical and Environmental Engineering, Universidad Nacional de Colombia - Sede Bogotá, Carrera 45 No 26-85, Bogotá, Colombia; Centro de Excelencia en Cannabis y Agronegocios, Universidad Nacional de Colombia, Colombia.
Grupo de Procesos Químicos y Bioquímicos, Department of Chemical and Environmental Engineering, Universidad Nacional de Colombia - Sede Bogotá, Carrera 45 No 26-85, Bogotá, Colombia.
J Chromatogr A. 2025 Aug 30;1757:466173. doi: 10.1016/j.chroma.2025.466173. Epub 2025 Jun 25.
In this study, a method was developed for the separation of tetrahydrocannabinol (THC) from a Cannabis extract to obtain a THC-free product that meets regulatory and commercial specifications for large-scale production. Considering Colombia's regulations and pharmaceutical restrictions on certain solvents, heptane, ethanol, and water were selected for this study. Process simulation software (ASPEN Plus V14) was used to generate a ternary phase diagram and identify suitable solvent systems for the separation of THC from cannabis extract. In this diagram, the biphasic (liquid-liquid) region was determined, and within it, the low-polarity zone (characterized by low water content) was delineated. Four heptane/ethanol/water (HEtWat) solvent systems were preselected: I: 4.6/3.5/1, II: 7.2/5.6/1, III: 16.2/10.4/1, and IV: 4/4/1 (v/v/v). These systems were evaluated based on the THC partition coefficient (K). Two solvent systems were selected for laboratory-scale tests using a Gilson CPC 250 unit. Among them, the heptane/ethanol/water system 4.6/3.5/1 (v/v/v) was chosen for method development at industrial scale using a Rothacrom rCPC system. Additionally, two laboratory-scale tests demonstrated the method's viability to: (1) separate THC from mother liquor (a byproduct resulting from the crystallization of cannabidiol (CBD)) yielding a THC-free product enriched in minor cannabinoids (a key feature of mother liquor); and (2) purify THC from a refined extract (distillate) enriched in this cannabinoid. several tests was performed to determine the maximum mass of full-spectrum (FS) Cannabis extract that could be processed, achieving sufficient THC separation to comply with regulatory limits (THC < 0.05 %). The process yielded 613 g of THC-free extract, referred to as broad spectrum (BS), containing 85 % CBD and 0.02 % THC, from 800 g of FS in 9.5 h, resulting in an operational efficiency of 77 % (613 g BS / 800 g FS). A total of 97.06 % of cannabichromene (CBC) was recovered in the residual fraction, indicating strong retention of this cannabinoid by the stationary phase. Fractions 9 and 10 contained 85.3 % (w/w) THC. These THC- and CBC-rich fractions are proposed for further isolation and potential applications in medical research.
在本研究中，开发了一种从大麻提取物中分离四氢大麻酚（THC）的方法，以获得符合大规模生产监管和商业规格的无THC产品。考虑到哥伦比亚对某些溶剂的法规和制药限制，本研究选择了庚烷、乙醇和水。使用过程模拟软件（ASPEN Plus V14）生成三元相图，并确定从大麻提取物中分离THC的合适溶剂体系。在该图中，确定了双相（液-液）区域，并在其中划定了低极性区域（以低含水量为特征）。预先选择了四种庚烷/乙醇/水（HEtWat）溶剂体系：I：4.6/3.5/1，II：7.2/5.6/1，III：16.2/10.4/1，IV：4/4/1（v/v/v）。根据THC分配系数（K）对这些体系进行评估。选择了两种溶剂体系，使用吉尔森CPC 250装置进行实验室规模测试。其中，庚烷/乙醇/水体系4.6/3.5/1（v/v/v）被选用于使用Rothacrom rCPC系统进行工业规模的方法开发。此外，两项实验室规模测试证明了该方法的可行性：（1）从母液（大麻二酚（CBD）结晶产生的副产品）中分离THC，得到富含次要大麻素的无THC产品（母液的一个关键特征）；（2）从富含该大麻素的精制提取物（馏出物）中纯化THC。进行了多项测试，以确定可处理的全谱（FS）大麻提取物的最大质量，实现足够的THC分离以符合监管限值（THC<0.05%）。该工艺在9.5小时内从800克FS中得到613克无THC提取物，称为广谱（BS）提取物，含有85%的CBD和0.02%的THC，操作效率为77%（613克BS/800克FS）。在残留馏分中总共回收了97.06%的大麻色烯（CBC），表明该大麻素被固定相强烈保留。第9和第10馏分含有85.3%（w/w）的THC。这些富含THC和CBC的馏分建议进一步分离，并在医学研究中具有潜在应用。
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