The purification of natural products can be achieved by various techniques, including single- and multi-column liquid chromatography. However, the development of efficient, fast and cost-effective methods for the purification of natural products from samples such as natural extracts remains a difficult and challenging task due to the complexity of the matrix. In contrast to conventional purification methods such as distillation, preparative chromatography uses less energy, consumes less water and chemicals while achieving higher yields1.
In this application, a SMB process for the purification of CBD (cannabidiol) from a CBD-rich cannabis extract was established. First, a sample preparation was carried out, followed by preliminary tests on the analytical system to design the starting parameters for the SMB process. Subsequently, different separation runs were tested on the SMB system to determine the optimal separation and purification parameters. The SMB process enabled the purification of approximately 95 mg CBD/cycle with a yield of 81 % and purity of 93%.
Fig. 1 Preparative fractionation of the cannabinoid peak (F1); wavelenght: 228 nm measured with ES II 100-10 C18 150 x 50 mm; 10 ml, 60 ml/min.
Fig. 3 Overload study in analytical scale. Sample: purified and evaporated CBD-rich cannabis extract; injection volumes blue: 5 μl; red: 10 μl, black: 20 μl; green: 50 μl; yellow: 100 μl; wavelenght: 228 nm measured with ES II 100-15 C18 250 x 8 mm; 4 ml/
Fig. 5 Screenshot of the Purity MCC - SMB calculator with the SMB start parameters and the separation triangle for linear isotherms.
Fig. 11 Chromatograms of the three outlets for cycle 15 and the higher concentrated sample. 1: CBC, 2: Δ9-THC, 3: CBC. MO2; black: sample; blue: raffinate; red: extract; green: waste; wavelenght: 228 nm measured with ES II 100-15 C18 250 x 4 mm; 10 μl; 1
Fig. 13 System setup SMB; left: Detectors, flow meter; middle from top to bottom: Eluent tray with bottles, assistant 1 with manual valve, assistant 2 with measuring cell, manual valve and column holder, assistant 3 with measuring cell and manual valve, a
| Method | SMB |
|---|---|
| Mode | RP |
| Substances | Cannabidiol (CBD), Cannabichromene (CBC), (−)-trans-Δ9-tetrahydrocannabinol (∆9-THC) |
| Key words | SMB, continuous chromatography, preparative chromatography, RP, purification of natural products, method development, separation |
| CAS number | 13956-29-1, 20675-51-8, 1972-08-3 |
| Version | Version 1 / 12/2024 |
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