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Method for extracting and purifying macamide monomer compound from maca

A technology for purifying macamide and compounds, which is applied in the separation/purification of carboxylic acid amide, organic chemistry, etc., can solve the problems of no mass preparation method of macamide monomer compounds, etc., and achieve low cost, simple operation and simple process Effect

Active Publication Date: 2017-05-03
JIANGSU HUIBO BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] At present, the extraction method of plant Maca composition main report is to adopt plant Maca as raw material to carry out the extraction of active ingredient, can make Maca alkaloid (preparation method and application of a kind of Maca alkaloid of Chinese patent (CN103275012)), Maca polysaccharide (Chinese patent (CN102898534) a kind of method for extracting and refining Maca polysaccharide) and Maca effective active ingredient (Chinese patent (CN1166387) Maca active ingredient extraction method), etc., but there is no macamide monomer compound at present Mass preparation method

Method used

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  • Method for extracting and purifying macamide monomer compound from maca

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Plant maca is crushed into 40-60 mesh maca powder, weighs 120 grams of maca powder, puts it into a multi-stage countercurrent extraction device, and then adds 1200ml of 80% ethanol-acetic acid aqueous solution for countercurrent extraction for 5 hours, after extraction Filter, concentrate under vacuum (0.05-0.1MPa), and concentrate under reduced pressure at about 50°C to obtain 17.8 grams of crude macamide.

[0024] Take a glass chromatographic column with a column length of 450 mm and an internal diameter of 45 mm, and install 350 ml of D101 macroporous adsorption resin, load the above-mentioned crude product of macamide on the top of the column, and then use mobile phases of 50%, 60%, and 70% respectively. %, 80%, 90% ethanol-water solution for gradient elution, TLC plate tracking, concentration under vacuum (0.05-0.1MPa), and water with absolute ethanol to obtain 64mg N-benzyl-5-oxo -6E, 8E-octadecadienamide (purity 97.3%), 31mg N-benzyl-hexadecanamide (purity 95.8%)...

Embodiment 2

[0033] Plant maca is pulverized into 40-60 mesh maca powder, takes by weighing 120 grams of plant maca powder, packs in the multistage countercurrent extraction device, then adds 80% ethanol-glycine aqueous solution of 1200ml, carries out multistage countercurrent extraction 4 After 1 hour, the extract was filtered, and the filtrate was concentrated under vacuum (0.05-0.1 MPa), and concentrated under reduced pressure at about 55° C. to obtain 16.5 grams of crude plant macamide.

[0034] Take a glass chromatographic column with a column length of 450mm and an inner diameter of 45mm, and install 250ml of DM301 macroporous adsorption resin, load the above-mentioned crude macamide sample on the top of the column, and then use mobile phases of 50%, 60%, and 70%, 80%, 90% ethanol-water solution for gradient elution, followed by TLC plate, concentrated under vacuum (0.05-0.1MPa), and carried water with absolute ethanol to obtain 57mg N-benzyl-5-oxo Generation-6E,8E-octadecadienamide ...

Embodiment 3

[0036] The plant maca medical material is crushed into 40-60 mesh maca powder, 120 grams of macamide powder is weighed, packed into a multistage countercurrent extraction device, and then 1200ml of 80% ethylene propanol-phosphoric acid aqueous solution is added to carry out multiple extractions at room temperature. Stage countercurrent extraction for 2 hours, the extract was taken out and filtered, the filtrate was concentrated under vacuum (0.05-0.1MPa), and concentrated under reduced pressure at about 30°C to obtain 14.3 grams of crude macamide.

[0037] Take a glass chromatographic column with a column length of 450mm and an inner diameter of 45mm, install 350ml DA-201 macroporous adsorption resin, load the above-mentioned crude product of macamide on the top of the chromatographic column, and then use 50% and 60% mobile phase respectively , 70%, 80%, and 90% ethanol-water solution for gradient elution, followed by TLC plate, concentrated under vacuum (-0.6-0.1MPa), and carr...

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Abstract

The invention discloses a method for extracting and purifying monomeric macamide compounds from maca. The method comprises the steps of smashing plant maca into maca powder, adding an alcohol-acid water solution to carry out multistage countercurrent extraction, and carrying out vacuum concentration after filtering an extracting solution to obtain crude macamide; and separating and purifying by using macroporous adsorption resin, carrying out gradient elution, collecting an eluant, and respectively carrying out vacuum concentration to obtain the monomeric macamide compounds. Because the macamide compound has favorable and stable physical properties under a weak acid condition, a multistage countercurrent extraction method is carried out by using the alcohol-acid water solution, and the alcohol-acid water solution can be used for protecting effective components of macamide during extraction and greatly increasing the extraction ratio of the effective components in maca plants; the macroporous adsorption resin can be repeatedly utilized; the alcohol-acid water solution serving as a solvent is economical and practical; the high-purity monomeric macamide compounds can be conveniently and efficiently obtained, and the purity of each monomeric compound is up to more than 95%; and the method is simple in process, simple and convenient to operate, low in cost and suitable for batch production.

Description

technical field [0001] The invention relates to a method for extracting and purifying a monomer compound of macamide from new resource food maca, belonging to the technical field of traditional Chinese medicine phytochemistry. Background technique [0002] Maca, also known as Maca (Maca, Lepidium meyemii Walp), belongs to the genus Cruciferae (Cruciferae). In mountainous areas, local people mainly use it as food and as traditional medicine. In 1982, with the efforts of international organizations such as FAO (Food and Agriculture Organization of the United Nations) and IPGRI (International Plant Genetic Resources Research Institute), Maca was widely promoted worldwide, and pointed out that Maca is a nutritionally safe food that can solve many diseases. health problems caused by nutritional deficiencies. In 2011, the Chinese government approved maca powder as a new resource food. Maca contains nutritional and active ingredients such as macamides and macaenes. It is a pure ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/24C07C233/18C07C235/76C07C235/74
Inventor 徐德锋
Owner JIANGSU HUIBO BIOTECH
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