Method for preparing high-purity cannabidiol by combining macroporous resin enrichment with dynamic axial compression column system

A technology of axial compression and macroporous resin, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of long extraction time, low purity, low yield, etc., and achieve short separation cycle, reduce Environmental pollution, high efficiency effect

Pending Publication Date: 2020-10-30
黑龙江阳光工业大麻研究院
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the problems of low yield, low purity and long extraction time of existing cannabidiol extraction methods, the present invention provides a method for preparing high-purity cannabidiol by enriching macroporous resin combined with dynamic axial compression column system , the technical scheme adopted is as follows:

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  • Method for preparing high-purity cannabidiol by combining macroporous resin enrichment with dynamic axial compression column system

Examples

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Embodiment 1

[0034] This embodiment provides a method for preparing high-purity cannabidiol by enriching a macroporous resin combined with a dynamic axial compression column system. The method is carried out according to the following steps:

[0035] Step 1: drying the tidbits and leaves of industrial hemp at 55°C for 8 hours until the water content is between 3% and 5%, crushing and passing through a 100-mesh sieve to obtain industrial hemp powder;

[0036] Step 2: Add 20 times the volume of 75% (volume percent concentration) ethanol solution to the industrial hemp powder, heat and reflux for extraction 3 times, each time for 1.5 hours, combine the extracts, centrifuge or filter, and recover the extraction solvent under reduced pressure. Carry out double-effect concentration, after concentration, adjust the pH value to 5.0-6.0 to get the column solution, pass the column solution through the macroporous adsorption resin chromatography column at a flow rate of 2BV / h, and the column solution ...

Embodiment 2

[0040] This embodiment provides a method for preparing high-purity cannabidiol by enriching a macroporous resin combined with a dynamic axial compression column system. The method is carried out according to the following steps:

[0041] Step 1: drying the tidbits and leaves of industrial hemp at 60°C for 6 hours until the water content is between 3% and 5%, crushing them and passing them through an 80-mesh sieve to obtain industrial hemp powder;

[0042] Step 2: Add 16 times the volume of 50% (volume percent concentration) methanol solution to the industrial hemp powder, heat and reflux for extraction 3 times, each time for 2 hours, combine the extracts, then concentrate after centrifugation or filtration, and adjust the pH after concentration When the value reaches 4.0-5.0, the column solution is obtained. Pass the column solution through the macroporous adsorption resin chromatography column at a flow rate of 3BV / h, and the column solution is 1:10 according to the ratio of s...

Embodiment 3

[0049] This embodiment provides a method for preparing high-purity cannabidiol by enriching a macroporous resin combined with a dynamic axial compression column system. The method is carried out according to the following steps:

[0050] Step 1: drying the tidbits and leaves of industrial hemp at 70°C for 6 hours until the water content is between 3% and 5%, crushing and passing through a 60-mesh sieve to obtain industrial hemp powder;

[0051] Step 2: Add 12 times the volume of 80% (volume) methanol solution to the industrial hemp powder, heat and reflux for extraction twice, each time for 3 hours, combine the extracts, filter the obtained filtrate to recover the extraction solvent under reduced pressure, adjust after concentration When the pH value reaches 6.8, the column solution is obtained, and the column solution is passed through the macroporous adsorption resin chromatography column at a flow rate of 2BV / h, and the column solution is 1:9 according to the ratio of solids...

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Abstract

The invention discloses a method for preparing high-purity cannabidiol by combining macroporous resin enrichment with a dynamic axial compression column system, and belongs to the technical field of natural medicine preparation. The method comprises the following steps: drying floccules and leaves of industrial hemp, crushing and sieving; obtaining industrial hemp powder, heating, refluxing and extracting to prepare an upper column solution; passing through a macroporous adsorption resin chromatographic column; performing post-water elution, recovering the solvent from the eluent, concentrating to obtain a cannabidiol primary extract, adding methanol and crude silica gel, uniformly stirring, drying to obtain a loading sample, treating the loading sample by using a dynamic axial compressioncolumn system, carrying out gradient elution by using a mobile phase, concentrating the eluent, filtering, recovering the mobile phase solvent, and drying to obtain cannabidiol crystals. The method has the advantages of high yield, high cannabidiol purity and short extraction time, solves the problems of low production efficiency, low purity and long extraction time in the existing cannabidiol extraction technology, and is suitable for industrial extraction of cannabidiol.

Description

technical field [0001] The invention relates to a method for preparing high-purity cannabidiol by macroporous resin enrichment combined with a dynamic axial compression column system, which belongs to the technical field of natural medicine preparation. Background technique [0002] Hemp plants have a long history of planting in China. In ancient times, hemp plant fibers were mainly used to make and process ropes, fishing nets, clothing and paper-making raw materials, and hemp seeds were used to extract oil and food industries. Industrial hemp (Cannabissativa) is fundamentally different from traditional poisonous marijuana. According to the clear regulations of the United Nations in 1988, industrial hemp refers to those that do not have the value of extracting addictive components (THC) or are directly smoked as drugs, and are exclusively for industrial use. The content of tetrahydrocannabinol (THC) in the tidbits and leaves of the raw hemp and the industrial hemp in the gro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/70C07C37/84C07C39/23C07C37/68
CPCC07C37/70C07C37/84C07C37/68C07C39/23
Inventor 刘欣曹亮
Owner 黑龙江阳光工业大麻研究院
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