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A method for efficiently preparing macamide monomer from maca

A technology for macamide and maca, which is applied in the field of efficient preparation of macamide monomers, can solve the problems of difficulty in ensuring high purity of macamide monomers, low recovery rate of macamide, and unpreparedness, etc. The effect of short cycle, large preparation and high feasibility

Active Publication Date: 2018-07-10
UNO SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The currently disclosed methods for extracting Maca components mainly obtain extracts mainly containing Maca amide, such as the patent "A Preparation Process of Maca Extract" (Application No.: CN201310400554.6), "A Maca Extract". Refining method of amide" (application number: CN201410230461.8), "a preparation method of macamide" (application number: CN201410450542.9), "a kind of maca extract, its preparation method and its use" (application No.: CN201310462943.1), and the macamide monomer prepared by the patent "Method for Extracting and Purifying Maca Amide Monomer Compound from Maca" (Application No.: CN201510568193.5) is difficult to guarantee its high purity. The preparation amount is small, the recovery rate of macamide is low, and the 4 kinds of macamide monomers prepared by the present invention have not been prepared

Method used

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  • A method for efficiently preparing macamide monomer from maca
  • A method for efficiently preparing macamide monomer from maca

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Get 5897.3g of maca root, crush it through a 20-mesh sieve, and put it into supercritical CO 2 In the extraction kettle, at a temperature of 45°C and an extraction pressure of 30MPa, CO 2 The flow rate is 200L / h, the extraction is 2h, and 22g of maca extract is obtained.

[0033] The maca extract was separated by normal phase silica gel column chromatography by dry mixing and wet column packing, gradient elution was carried out with n-hexane-ethyl acetate, and the main fraction containing macamide was collected for later use. Use high-efficiency countercurrent chromatography equipment to separate the main macamide-containing fraction, mix n-hexane-ethyl acetate-methanol-water in a volume ratio of 6:1:5:1, and separate after static layering. The above phase is The stationary phase, the lower phase is the mobile phase, the single injection volume is 1.01g, the injection concentration is 50mg / ml (dissolved in the upper phase), the flow rate of the mobile phase is 10ml / min...

Embodiment 2

[0037] Get 6000g of maca root, crush it through a 20-mesh sieve, and put it into supercritical CO 2 In the extraction kettle, at a temperature of 50°C and an extraction pressure of 28MPa, CO 2 Flow rate is 300L / h, extraction is 2h, obtains Maca extract 23g.

[0038] The maca extract was mixed by dry method and packed by wet method for normal phase silica gel column chromatography, and gradient elution was carried out by n-hexane-acetone, and the fraction mainly containing macamide was collected for later use. Use high-efficiency countercurrent chromatography equipment to separate the main macamide-containing fraction, mix n-hexane-ethyl acetate-methanol-water in a volume ratio of 7:2:5:1, and separate after standing and layering. The above phase is The stationary phase, the lower phase is the mobile phase, the single injection volume is 2.0g, the injection concentration is 70mg / ml (dissolved in the upper phase), the flow rate of the mobile phase is 10ml / min, the rotation spee...

Embodiment 3

[0042] Take 6150g of maca root, crush it through a 10-mesh sieve, and put it into CO 2 In a supercritical extraction kettle, with a temperature of 48°C and an extraction pressure of 29MPa, CO 2 Flow rate is 250L / h, extract 3h, obtain maca extract 23.5g.

[0043] The maca extract was mixed by dry method and packed by wet method for normal phase silica gel column chromatography, and petroleum ether-ethyl acetate was used for gradient elution, and the main fraction containing macamide was collected for later use. Use high-efficiency countercurrent chromatography equipment to separate the main macamide-containing fraction, mix n-hexane-ethyl acetate-methanol-water in a volume ratio of 8:2:5:1, and separate after standing and layering. The above phase is The stationary phase, the lower phase is the mobile phase, the single injection volume is 5.0g, the injection concentration is 100mg / ml (dissolved in the upper phase), the flow rate of the mobile phase is 10ml / min, the rotation sp...

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Abstract

The invention discloses a method for efficiently preparing macamides monomers from Lepidium meyenii, comprising the steps: crushing and screening tuber of Lepidium meyenii to obtain Lepidium meyenii powder, and collecting Lepidium meyenii extract by supercritical CO2 extraction; separating by normal-phase silica-gel column chromatography; subjecting fraction obtained by separation by normal-phase silica-gel column chromatography to separation by efficient countercurrent chromatography. The macamides monomers prepared herein are, respectively, N-benzyl-hexadecanamide, N-benzyl-9Z-octadecenoamide, N-benzyl-(9Z,12Z)-octadecadienamide, N-(3-methoxy-benzyl)-(9Z,12Z)-octadecadienamide, and N-(3-methoxy-benzyl)-(9Z,12Z,15Z)-octadecatrienamide. The method is low in cost, simple to perform, highly feasible and short in preparation cycle, the activity of obtained macamides is completely retained, and the method is suitable for engineering production.

Description

【Technical field】 [0001] The invention relates to the preparation of maca bioactive components, in particular to a method for efficiently preparing macamide monomers from maca. 【Background technique】 [0002] Maca (Maca), also known as Peruvian ginseng, maka, etc., is a South American annual or biennial herb belonging to the genus Lepidium meyenii Walp. of the Cruciferae family. Maca is traditionally used as food and herbal medicine to enhance energy, fight fatigue, improve sexual function, enhance fertility, treat menopausal syndrome in women, etc. As a symbolic component of maca, macamides can improve fertility, enhance energy, and have a significant effect on balancing human hormone secretion, so maca is also known as a natural hormone engine. [0003] The currently disclosed methods for extracting Maca components mainly obtain extracts mainly containing Maca amide, such as the patent "A Preparation Process of Maca Extract" (Application No.: CN201310400554.6), "A Maca Ex...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/24C07C233/05C07C233/09C07C233/20
CPCC07C231/24C07C233/05C07C233/09C07C233/20Y02P20/54
Inventor 梁耀光张天佑王义娜吕巧莉周丽敏
Owner UNO SCI CO LTD
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