Cannabinoid Purification via Cyclohexane CPC
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Solution Overview
Problem
Current methods for extracting cannabinoids, such as THC and CBD, from cannabis extracts using Centrifugal Partition Chromatography (CPC) face challenges in achieving high purity and yield, with prior art methods achieving maximum purities of around 93.1% and requiring multiple steps, while also using neurotoxic solvents like hexane.
Innovation Solution
A method utilizing a two-phase solvent system with cyclohexane, n-heptane, or iso-octane as the stationary phase and acetonitrile as the mobile phase, with optional addition of t-butyl methyl ether, which enhances separation performance, achieving purities over 95% and reducing the need for additional chromatographic steps, and allows for easy renewal of the stationary phase.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If hexane is used as the stationary phase in CPC, then the separation process can be performed, but the purity achieved is limited to maximum 93.1% and hexane is neurotoxic
Solution Approach 1:
The patent changes the chemical parameters of the stationary phase by replacing hexane with cyclohexane, n-heptane, or iso-octane. This substitution maintains the functional properties needed for separation while eliminating the neurotoxicity issue, and simultaneously improves purity from 93.1% to over 95%
Solution Approach 2:
The patent treats the stationary phase as a disposable component that can be easily renewed by distillation. Each run completely renews the stationary phase, eliminating the need for complex regeneration processes and allowing simple replacement of toxic solvents with safer alternatives
2Manufacturing precision
If a two-phase system based on hexane is used, then separation can be achieved, but additional chromatographic steps are required and yields are low
Solution Approach 1:
The patent modifies the phase system parameters by using cyclohexane, n-heptane, or iso-octane as stationary phase with acetonitrile as mobile phase. This parameter change achieves purities over 95% in a single step, eliminating the need for multiple chromatographic steps and significantly increasing yield
Solution Approach 2:
The patent extracts and removes the problematic hexane-based system and replaces it with an improved solvent system. The new system extracts cannabinoids with higher efficiency in a single step, taking out the need for additional purification steps
3Productivity
If the stationary phase is used multiple times, then process efficiency is maintained, but deposits accumulate requiring regeneration or removal of interfering components
Solution Approach 1:
The patent treats the stationary phase as a disposable component that is completely renewed after each run through simple distillation. This approach maintains high process efficiency while ensuring consistent purity over 95%, as each run starts with a fresh, deposit-free stationary phase
Solution Approach 2:
The patent discards the used stationary phase after each run and recovers it through simple distillation for complete renewal. This process eliminates deposit accumulation and interfering components, maintaining both high productivity and purity without complex regeneration procedures
Applied Scientific Principles
This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.
Function Achieved in This Case
This method achieves high purity and yield of cannabinoids, often exceeding 95%, with reduced process stages and minimal eluent consumption, enabling efficient industrial-scale extraction with minimal solvent toxicity and no deposition on the stationary phase.
Implementation Method 1
CPC is a liquid-liquid chromatography method that typically uses a two-phase solvent system. In these chambers, arranged directly one after the other, the substances contained in the plant extract are distributed between the mobile and stationary phases.
Implementation Method 2
The partition coefficient K of the desired substance between the two phases should be between 0.7 and 4.5. At lower K values, the substance elutes too quickly, making separation impossible. At higher K values, however, the retention time becomes too long
Implementation Method 3
The system is set into rapid rotation (up to 2,500 rpm) during the separation process. This not only retains the desired phase in the CPC rotor, depending on the flow direction, but also accelerates the separation of the two phases through centrifugal force.
Implementation Method 4
The density and viscosity of cyclohexane, n-heptane and iso-octane are greater than the density/viscosity of n-hexane, so that a more stable two-phase system is produced compared to a second mobile phase such as acetonitrile, for example, enabling better retention of the stationary phase
Data Source
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AI summary
The invention relates to the isolation and purification of cannabinoids by means of centrifugal partition chromatography.