Method for extracting and separating high-purity cannabidiol from low-content industrial hemp floral leaves

A technology of cannabidiol and industrial hemp, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of poor separation effect of cannabinoids, poor production of complete sets, large investment in equipment, etc., and achieve improvement The effects of high sample load, increased content, and high reusability

Active Publication Date: 2020-07-31
SUNRESIN NEW METERIALS CO LTD XIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problems of low extraction rate in the production of existing industrial hemp leaves, poor production of complete sets, large investment in equipment, and poor separation effect of cannabinoids other than cannabidiol, the present invention provides a method of extracting from low-content industrial hemp leaves. Method for extracting and purifying high-purity cannabidiol and other cannabinoids

Method used

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  • Method for extracting and separating high-purity cannabidiol from low-content industrial hemp floral leaves
  • Method for extracting and separating high-purity cannabidiol from low-content industrial hemp floral leaves
  • Method for extracting and separating high-purity cannabidiol from low-content industrial hemp floral leaves

Examples

Experimental program
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Effect test

Embodiment 1

[0107] Extraction: 500g of industrial hemp flowers and leaves with a CBD content of 0.6% (w / w), crushed to an average particle size of 1mm, passed through a sieve to obtain 400g of powder, added 2.4L of pure water, stirred, heated to 70°C, and kept for 4h , filter; add 2.4L 30% (V / V) ethanol to the filter residue, stir, heat up to 70°C, keep warm for 4h, filter; add 2L 90% (V / V) ethanol to the filter residue, stir, heat up to 70°C , keep warm for 4 hours, filter, and collect the filtrate; then add 2L of 90% (V / V) ethanol to the filter residue, stir, heat up to 70°C, keep warm for 4 hours, filter, and combine the filtrates to obtain 4L of extract. 45°C, 100mbar, concentrated to 0.26L by rotary evaporation. The concentration of CBD in the suspension after liquid phase detection and concentration is 8.8g / L, and the extraction rate is 95.3%. figure 1 .

[0108] Adsorption and analysis of macroporous resin: 45mlLX-T83 (produced by Xi'an Lanxiao Technology New Materials Co., Ltd.)...

Embodiment 2

[0112] Extraction: 500g of industrial hemp leaves with CBD content of 0.5% (w / w), crushed to an average particle size of 0.5mm, added 3.2L of purified water, stirred, heated to 20°C, kept for 3.5h, filtered; poured into the filter residue Add 3.2L 10% (V / V) methanol, stir, heat up to 20°C, keep warm for 3.5h, filter; add 3.2L 90%(V / V) methanol to the filter residue, stir, heat up to 40°C, keep warm for 2h, Filter and collect the filtrate; then add 3.2L of 90% (V / V) methanol to the filter residue, stir, heat up to 40°C, keep warm for 2h, filter, and combine the filtrates to obtain 6.4L of extract. 45°C, 100mbar, concentrated to 0.52L by rotary evaporation. The concentration of CBD in the suspension after liquid phase detection was 4.6g / L, and the extraction rate was 96.2%.

[0113] Adsorption and analysis of macroporous resin: 45ml of LX-T83 (produced by Xi'an Lanxiao Technology New Material Co., Ltd.) macroporous resin is wet-packed with 40% (V / V) methanol aqueous solution, t...

Embodiment 3

[0117] Extraction: 500g of industrial hemp flowers and leaves with a CBD content of 1% (w / w), crushed to an average particle size of 1mm, add 4L of pure water, stir, heat up to 30°C, keep warm for 3h, filter; add 4L10 to the filter residue % (V / V) n-propanol, stir, heat up to 30°C, keep warm for 3h, filter; add 4L 95% (V / V) n-propanol to the filter residue, stir, heat up to 50°C, keep warm for 2h, filter, Collect the filtrate; add 4L of 95% (V / V) n-propanol to the filter residue, stir, heat up to 50°C, keep warm for 2h, filter, and combine the filtrates to obtain 8L of extract. 45°C, 100mbar, concentrated to 0.56L by rotary evaporation. The concentration of CBD in the suspension after liquid phase detection and concentration was 8.5g / L, and the extraction rate was 95.2%.

[0118] Adsorption analysis of macroporous resin: 45ml LX-22 (produced by Xi'an Lanxiao Technology New Materials Co., Ltd.) macroporous resin is wet-packed with 40% (V / V) n-propanol aqueous solution, and the...

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Abstract

The invention discloses a method for extracting and separating high-purity cannabidiol (CBD) from low-content industrial hemp floral leaves. The method adopts the modes of digestion, macroporous resinadsorption and desorption, reverse chromatography and crystallization to finally obtain a cannabidiol pure product with the purity of 99% or above. In order to separate other cannabinoids, extractionand decoloration processes can be added between the digestion process and the macroporous resin adsorption and desorption process, and a polymer reversed-phase filler is used for reversed-phase chromatography, so that cannabidivarin (CBDV), cannabinol (CBN) and tetrahydrocannabinol (THC) in the floral leaves can be separated. The method disclosed by the invention is high in digestion, extractionand decoloration process yield and high in impurity removal rate; the macroporous resin and reversed-phase column chromatography have the advantages of high loading capacity and favorable separation effect. Requirements of development of a plurality of industrial hemp products are met, and the method has great application advantages in the pharmaceutical field and is suitable for industrial popularization.

Description

technical field [0001] The invention relates to a method for extracting and separating high-purity cannabidiol from low-content industrial hemp flowers and leaves, and belongs to the technical field of plant extraction and purification. [0002] technical background [0003] Cannabidiol (English name: cannabidiol, referred to as CBD) is a pure natural ingredient extracted from the cannabis plant. The molecular formula of cannabidiol is C 21 h 30 o 2 , the properties are white to light yellow viscous or crystal, melting point 66℃~67℃, almost insoluble in water, soluble in ethanol, methanol, ether, benzene, chloroform and other organic solvents. Cannabidiol has the effect of blocking the adverse effects of certain polyphenols on the human nervous system, and has a series of physiologically active functions such as blocking breast cancer metastasis, treating epilepsy, anti-rheumatoid arthritis, and anti-insomnia. Sclerosis has a good effect, and the future application prospe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/23C07C37/68C07C37/82C07C37/84C07C37/86
CPCC07C37/685C07C37/82C07C37/84C07C37/86C07C2601/16C07C39/23Y02P20/54
Inventor 张赪高月静任超鑫智旭亮贾晓妮刘琼智彩辉
Owner SUNRESIN NEW METERIALS CO LTD XIAN
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