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A method of extracting sinigrin

A technology of sinigrin and extract, which is applied in the field of preparation of active ingredients in plants, can solve the problems of easy decomposition or destruction, temperature decomposition influence, instability, etc., and achieve the effect of simple and easy to control and low production cost

Active Publication Date: 2017-03-15
GUILIN NATURAL INGREDIENTS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, due to the nature of sinigrin itself and the fact that sinigrin is easily destroyed during the extraction and purification process (sigrin is a glucosinolate, it is unstable in acid and alkali, it is easy to decompose or destroy, and at the same time when there are other metals The existence of ions (such as iron, zinc, copper, etc.) is also easy to destroy, and the temperature also has a great influence on its decomposition) making it difficult to separate and purify to obtain high content of sinigrin

Method used

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  • A method of extracting sinigrin
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1) Take 100kg of dried mustard seeds (the content of sinigrin is 3.3%, HPLC method, the same below), pulverize, reflux extract with 50v / v% ethanol equivalent to 8 times the weight of the raw material for 2h, filter, and reuse the residue Reflux extraction with 10 times the weight of the raw material and 50v / v% ethanol for 1.5h, filter, combine the extracts, extract the obtained extracts under reduced pressure to recover ethanol, centrifuge, and collect the supernatant;

[0020] 2) The supernatant was extracted twice with a mixed solvent (the volume ratio of ethyl acetate to methanol was 5:1), and the organic phase (upper layer solution) was combined and collected, and then the solvent was recovered under reduced pressure to obtain a concentrated solution (6 Baume);

[0021] 3) Take the concentrated solution and apply it to 700B type anion exchange resin column chromatography, wash the resin column with water until the effluent is clear and colorless, then elute with 1.5w...

Embodiment 2

[0042] Example 1 was repeated, except that in step 2), the original mixed solvent (the volume ratio of ethyl acetate to methanol was 5:1) was replaced with a combination of petroleum ether and acetone at a volume ratio of 1:3.

[0043]4.10 kg of sinigrin extract was obtained from this example, and the obtained sinigrin extract was tested, the purity was 72.50%, and the recovery rate of raw material sinigrin was 90.08%.

Embodiment 3

[0045] Example 1 was repeated, except that, in step 3), the anion exchange resin type 700B was replaced with anion exchange resin type 700A.

[0046] 4.05 kg of sinigrin extract was obtained from this example, and the obtained sinigrin extract was tested, and the purity was 73.80%, and the recovery rate of raw material sinigrin was 90.57%.

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Abstract

The invention discloses a method for extracting high-content sinigrin. The method comprises the following steps: (1) by using Cruciferae Brassica plants including leaf mustard, Brassica oleracea or broccoli as raw materials, extracting with ethanol to obtain an extracting solution, recycling ethanol from the extracting solution, centrifuging, and collecting liquid supernatant; (2) extracting the liquid supernatant with a mixed solvent, collecting an organic phase, and recycling the solvent under reduced pressure to obtain a concentrated solution, wherein the mixed solvent is combination of one of ethyl acetate, diethyl ether and petroleum ether and methyl alcohol or acetone in volume ratio of (5-6):1; and (3) carrying out anion exchange resin column chromatography on the concentrated solution, washing with a resin column until the outflowing liquid is clear, eluting with alkaline liquid, concentrating an eluant, drying to obtain a sinigrin extract with the purity being more than or equal to 70%. According to the method, the mixed solvent with special ratio is used for extracting the liquid supernatant, and the specific 700A or 700B anion exchange resin column chromatography process is combined, and therefore, the sinigrin extract with the purity being more than or equal to 70 can be obtained.

Description

technical field [0001] The invention relates to a preparation method of active ingredients in plants, in particular to a method for extracting sinigrin. Background technique [0002] Existing studies have shown that a diet rich in cruciferous vegetables, such as broccoli, cauliflower, kale, and mustard greens, can reduce the incidence of many cancers. At present, it is agreed that the precursors of the important anticancer active ingredients of cruciferous plants are Glucosinolates. More than 120 different glucosinolates have been found in natural plants, and they exist in 11 different species of dicotyledonous angiosperms, the most important being the cruciferous family, all cruciferous plants can synthesize thio glucoside. Glucosinolates are found in the roots, stems, leaves and seeds of these plants, but mostly in the seeds. [0003] Sinigrin, also known as sinigrin, is one of the most studied aliphatic glucosinolates. The R group of sinigrin is allyl, so sinigrin is a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/14C07H1/08
CPCC07H1/08C07H15/14
Inventor 赵军杨文国李杰李元元罗勇为黄华凤
Owner GUILIN NATURAL INGREDIENTS CORP
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