CN102048791A - Method for preparing sinigrin extract - Google Patents
Method for preparing sinigrin extract Download PDFInfo
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- CN102048791A CN102048791A CN2009101145149A CN200910114514A CN102048791A CN 102048791 A CN102048791 A CN 102048791A CN 2009101145149 A CN2009101145149 A CN 2009101145149A CN 200910114514 A CN200910114514 A CN 200910114514A CN 102048791 A CN102048791 A CN 102048791A
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Abstract
The invention discloses a method for preparing a sinigrin extract. The method comprises the following steps of: 1) extracting crucifer brassica mustard leaf, cabbage or broccoli serving as a raw material by using acetic acid, and centrifuging the extract to obtain supernate; 2) adding ethanol into the supernate, adjusting the ethanol concentration to be 80 to 85 percent, standing the solution for 1 to 1.5 hours, centrifuging the solution, and collecting secondary centrifugate; 3) concentrating the secondary centrifugate till no ethanol smell, filtering the concentrated centrifugate by using a ceramic film of 0.5 micron, concentrating the permeating solution until the volume of the permeating solution is 2 to 3 times weight of the raw materials to obtain concentrated permeating solution; and 4) filling the concentrated permeating solution into a macroporous resin column, collecting the effluent, eluting the effluent by using water in an amount which is 2 to 3 times weight of the resin, collecting eluant, combining the effluent and the eluant, and performing concentration and freeze drying to obtain the sinigrin extract. The method has simple process and is easy to operate, the sinigrin content of the obtained product can reach 20 to 40 percent, and the extraction rate of the sinigrin reaches over 80 percent.
Description
Technical field
The present invention relates to the preparation method of active component in the plant, be specifically related to the potassium myronate preparation method of extract.
Background technology
As far back as the eighties in 19th century, brassicaceous vegetable is eaten in the suggestion of international committee more, because brassicaceous vegetable can prophylaxis of cancer.China's crucifer kind mainly contains Brassica oleracea L. var. botrytis L., Caulis et Folium Brassicae capitatae, Caulis et Folium Brassicae capitatae, Radix Raphani, Caulis et Folium Brassicae junceae.Btassica is main edible vegetable in crucifer, and Brassica plants comprises Caulis et Folium Brassicae capitatae, Brassica oleracea L. var. botrytis L., turnip, burnt blue or green Caulis et Folium Brassicae capitatae, Brassica Oleracea Var.Acephala, Caulis et Folium Brassicae junceae etc.Epidemic data shows, is rich in the diet of brassicaceous vegetable, can reduce the sickness rate of many cancers as Caulis et Folium Brassicae capitatae, Brassica oleracea L. var. botrytis L., Caulis et Folium Brassicae capitatae etc.At present consistently think that the important anticancer active constituent precursor of crucifer is thioglycoside (Glucosinolates).Found the thioglycoside that kind more than 120 is different in natural plants, they are present in the dicotyledonous angiosperm of 11 different generas, the most important thing is Cruciferae, and all crucifers can both be synthesized thioglycoside.Thioglycoside is present in root, stem, leaf and the seed of these plants, but mainly is present in the seed.The content of thioglycoside in some crucifers accounts for 1% of dry weight greatly, and the content in some plant seeds reaches 10%.But, the changes of contents of thioglycoside in plant is very big, all there is difference in the different parts content of different cultivars, different growing environment and the different growth stages of same plant, same plant, is ripe plant or flower 10～100 times as the content of Glucorapha-nine in the Caulis et Folium Brassicae capitatae tender shoots.
All thioglycoside all contain glycosyl group, sulfate group and variable non-sugared side chain (R) by one and form.Based on the difference of R group, thioglycoside can be divided into 3 classes: aliphatic thioglycoside, aromatic series thioglycoside and indole thioglycoside.Potassium myronate (Sinigrin) is wherein study morely in the aliphatic thioglycoside a kind of, and the R group of potassium myronate is a pi-allyl, so potassium myronate also is the pi-allyl thioglycoside.Existing a lot of reports all are the methods of extracting thioglycoside from crucifer, " optimization of thioglycoside extraction process condition in the Caulis et Folium Brassicae junceae " (food and biotechnology journal of delivering as Tu Zongcai etc., in November, 2007, the 26th the 6th phase of volume, 9～12 pages) in the literary composition, obtaining the best process conditions of extracting thioglycoside from Caulis et Folium Brassicae junceae by single factor and orthogonal test is: the ethanol extraction of volumetric concentration 80% 2 times, the each extraction 20 minutes, extract 80 ℃ of temperature, the raw material solid-liquid ratio is (g/mL) 1: 7, granule size is 20 orders, and the extracted amount of thioglycoside is 22.146 μ mol/g in the Caulis et Folium Brassicae junceae.Yet there are no the relevant report of from crucifer, extracting preparation potassium myronate extract.
Summary of the invention
It is simple, easy to operate that the technical problem to be solved in the present invention provides a kind of technology, the potassium myronate preparation method of extract that extraction ratio is high.
Potassium myronate preparation method of extract of the present invention may further comprise the steps:
1) get raw material, pulverize, ethanol boils insulation and extracts, and extracting solution is centrifugal, collects supernatant; Wherein, described raw material is Cruciferae Brassica plants Caulis et Folium Brassicae junceae, Caulis et Folium Brassicae capitatae or Caulis et Folium Brassicae capitatae; Preferably select Caulis et Folium Brassicae junceae seed, cabbage seed or Caulis et Folium Brassicae capitatae alabastrum or tender shoots for use;
2) in supernatant, add ethanol, regulate wherein that concentration of alcohol is 80～85% (quality), placed 1～1.5 hour, centrifugal, collect secondary centrifuging liquid;
3) secondary centrifuging liquid is concentrated into does not have the alcohol flavor, and gained concentrates the ceramic membrane that centrifugal liquid is crossed 0.5 μ m, and permeate is concentrated into 2～3 times of raw material weight, must concentrate permeate;
4) concentrate permeate and advance macroporous resin column, collect effluent, with the water elution of 2～3 times of weight resins, collect eluent, merge effluent and eluent, concentrate, lyophilization promptly gets the potassium myronate extract.
In the step 1) of said extracted method, extracting with alcoholic acid volumetric concentration is 60～80%, and extraction time is 1～2 time, each 1～2 hour; When raw material is fresh feed, solid-liquid ratio during extraction is 1: 2～3 (W/V, promptly the raw material of 1 gram is with 2～3 milliliters extracting solution extraction), when raw material is dried feed, solid-liquid ratio during extraction is 1: 7～10 (W/V, promptly the raw material of 1 gram is with 7～10 milliliters extracting solution extraction).
Step 2) in, can be with supernatant concentration re-adjustment concentration of alcohol wherein to 0.5～3 times of raw material weight.
In the step 4), the model of macroporous resin is D101, DM130, DM132, DM312 or DM2.
Compared with prior art, the invention provides a kind of method for preparing the potassium myronate extract of from Cruciferae Brassica plants Caulis et Folium Brassicae junceae, Caulis et Folium Brassicae capitatae or Caulis et Folium Brassicae capitatae, extracting, this method is by carrying out high alcohol extraction, the supernatant after the extracting solution centrifugalize being carried out precipitate with ethanol and ceramic membrane filter to raw material, macro-molecular protein and polysaccharide in effectively removing wherein separate obtaining the potassium myronate extract again through macroporous resin column.This method technology is simple, easy to operate, and potassium myronate content can reach 20～40% in the product that obtains, and has avoided the oxidation of potassium myronate, and the extraction ratio of potassium myronate is more than 80%.
The specific embodiment
Embodiment 1 potassium myronate preparation method of extract may further comprise the steps:
1) gets exsiccant Caulis et Folium Brassicae junceae seed, pulverize, boiling insulation with the ethanol water that is equivalent to 8 times of raw material weights, 60% (v/v) extracted 2 hours, filter, the ethanol water that the residue reuse is equivalent to 10 times of raw material weights, 60% (v/v) extracted 1 hour, filtered merge extractive liquid,, centrifugal, collect supernatant;
2) add dehydrated alcohol in supernatant, concentration of alcohol is 80% (quality) in this mixed liquor, places 1 hour, and is centrifugal, collects secondary centrifuging liquid;
3) secondary centrifuging liquid is concentrated into does not have the alcohol flavor, and gained concentrates the ceramic membrane that centrifugal liquid is crossed 0.5 μ m, and permeate is concentrated into 2 times of raw material weight, must concentrate permeate;
4) concentrate permeate and advance D101 type macroporous resin column, collect effluent, with the distilled water eluting that is equivalent to 2 times of weight resins, collect eluent, merge effluent and eluent, and be concentrated into 60 Brix Scales, carry out drying with normal freeze-drying technology, promptly get the potassium myronate extract.
Measure with HPLC, the content of potassium myronate is 40% in the said extracted thing, and extraction ratio is 91%.
Embodiment 2 potassium myronate preparation method of extract may further comprise the steps:
1) get exsiccant cabbage seed, pulverize, boil insulation with the ethanol water that is equivalent to 10 times of raw material weights, 80% (v/v) and extracted 2 hours, filter, extracting solution is concentrated into 4 times of raw material weight, and is centrifugal, collects supernatant;
2) with supernatant concentration 0.5 times to raw material weight, to the ethanol water that wherein adds 95% (v/v), concentration of alcohol is 85% (quality) in this mixed liquor, places 1 hour, and is centrifugal, collects secondary centrifuging liquid;
3) secondary centrifuging liquid is concentrated into does not have the alcohol flavor, and gained concentrates the ceramic membrane that centrifugal liquid is crossed 0.5 μ m, and permeate is concentrated into 3 times of raw material weight, must concentrate permeate;
4) concentrate permeate and advance DM130 type macroporous resin column, collect effluent, with the distilled water eluting that is equivalent to 2 times of weight resins, collect eluent, merge effluent and eluent, and be concentrated into 60 Brix Scales, carry out drying with normal freeze-drying technology, promptly get the potassium myronate extract.
Measure with HPLC, the content of potassium myronate is 35% in the said extracted thing, and extraction ratio is 85%.
Embodiment 3 potassium myronate preparation method of extract may further comprise the steps:
1) gets the stem and leaf of fresh Caulis et Folium Brassicae junceae, be crushed to 20～30 orders, boiling insulation with the ethanol water that is equivalent to 3 times of raw material weights, 70% (v/v) extracted 2 hours, filter, the ethanol water that the residue reuse is equivalent to 2 times of raw material weights, 80% (v/v) extracted 2 hours, filtered, merge extractive liquid,, extracting solution is concentrated into 4 times of raw material weight, and it is centrifugal that cold back is put in taking-up, collects supernatant;
2) with supernatant concentration 1.5 times to raw material weight, again to the ethanol water that wherein adds 90% (v/v), concentration of alcohol is 82% (quality) in this mixed liquor, places 1.5 hours, and is centrifugal, collects secondary centrifuging liquid;
3) secondary centrifuging liquid is concentrated into does not have the alcohol flavor, and gained concentrates the ceramic membrane that centrifugal liquid is crossed 0.5 μ m, and permeate is concentrated into 3 times of raw material weight, must concentrate permeate;
4) concentrate permeate and advance DM312 type macroporous resin column, collect effluent, with the distilled water eluting that is equivalent to 2 times of weight resins, collect eluent, merge effluent and eluent, and be concentrated into 60 Brix Scales, carry out drying with normal freeze-drying technology, promptly get the potassium myronate extract.
Measure with HPLC, the content of potassium myronate is 30% in the said extracted thing, and extraction ratio is 88%.
Embodiment 4 potassium myronate preparation method of extract may further comprise the steps:
1) gets fresh Caulis et Folium Brassicae capitatae tender shoots, be crushed to 20～30 orders, boiling insulation with the ethanol water that is equivalent to 2 times of raw material weights, 75% (v/v) extracted 1 hour, filter, the ethanol water that the residue reuse is equivalent to 2 times of raw material weights, 60% (v/v) extracted 1.5 hours, filtered, merge extractive liquid,, extracting solution is concentrated into 5 times of raw material weight, and it is centrifugal that cold back is put in taking-up, collects supernatant;
2) with supernatant concentration 2.5 times to raw material weight, again to the ethanol water that wherein adds 95% (v/v), concentration of alcohol is 80% (quality) in this mixed liquor, places 1.3 hours, and is centrifugal, collects secondary centrifuging liquid;
3) secondary centrifuging liquid is concentrated into does not have the alcohol flavor, and gained concentrates the ceramic membrane that centrifugal liquid is crossed 0.5 μ m, and permeate is concentrated into 2 times of raw material weight, must concentrate permeate;
4) concentrate permeate and advance DM2 type macroporous resin column, collect effluent, with the distilled water eluting that is equivalent to 3 times of weight resins, collect eluent, merge effluent and eluent, and be concentrated into 60 Brix Scales, carry out drying with normal freeze-drying technology, promptly get the potassium myronate extract.
Measure with HPLC, the content of potassium myronate is 35% in the said extracted thing, and extraction ratio is 82%.
Claims (3)
1. potassium myronate preparation method of extract is characterized in that may further comprise the steps:
1) get raw material, pulverize, ethanol boils insulation and extracts, and extracting solution is centrifugal, collects supernatant; Wherein, described raw material is Cruciferae Brassica plants Caulis et Folium Brassicae junceae, Caulis et Folium Brassicae capitatae or Caulis et Folium Brassicae capitatae;
2) in supernatant, add ethanol, regulate wherein that concentration of alcohol is 80～85% (quality), placed 1～1.5 hour, centrifugal, collect secondary centrifuging liquid;
3) secondary centrifuging liquid is concentrated into does not have the alcohol flavor, and gained concentrates the ceramic membrane that centrifugal liquid is crossed 0.5 μ m, and permeate is concentrated into 2～3 times of raw material weight, must concentrate permeate;
4) concentrate permeate and advance macroporous resin column, collect effluent, with the water elution of 2～3 times of weight resins, collect eluent, merge effluent and eluent, concentrate, lyophilization promptly gets the potassium myronate extract.
2. potassium myronate preparation method of extract according to claim 1 is characterized in that: in the step 1), extracting with alcoholic acid volumetric concentration is 60～80%, and extraction time is 1～2 time, each 1～2 hour; When raw material was fresh feed, the solid-liquid ratio during extraction was 1: 2～3 (W/V), and when raw material was dried feed, the solid-liquid ratio during extraction was 1: 7～10 (W/V).
3. potassium myronate preparation method of extract according to claim 1 and 2 is characterized in that: in the step 4), the model of macroporous resin is D101, DM130, DM132, DM312 or DM2.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101145149A CN102048791B (en) | 2009-11-01 | 2009-11-01 | Method for preparing sinigrin extract |
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| CN2009101145149A CN102048791B (en) | 2009-11-01 | 2009-11-01 | Method for preparing sinigrin extract |
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| CN102048791B CN102048791B (en) | 2012-05-23 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327132A (en) * | 2014-10-23 | 2015-02-04 | 桂林莱茵生物科技股份有限公司 | Method for extracting high-content sinigrin |
| US11464247B2 (en) | 2006-09-07 | 2022-10-11 | Guilin Gfs Monk Fruit Corp. | Sweetening compositions and processes for preparing them |
| US11576412B2 (en) | 2016-10-24 | 2023-02-14 | Guilin Gfs Monk Fruit Corporation | Extracts from fruits of the Cucurbitaceae family, and methods of preparing thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100528891C (en) * | 2007-07-09 | 2009-08-19 | 浙江工商大学 | Method for separating and preparing glucose radish seeds glycosides from cauliflower seeds |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11464247B2 (en) | 2006-09-07 | 2022-10-11 | Guilin Gfs Monk Fruit Corp. | Sweetening compositions and processes for preparing them |
| CN104327132A (en) * | 2014-10-23 | 2015-02-04 | 桂林莱茵生物科技股份有限公司 | Method for extracting high-content sinigrin |
| US11576412B2 (en) | 2016-10-24 | 2023-02-14 | Guilin Gfs Monk Fruit Corporation | Extracts from fruits of the Cucurbitaceae family, and methods of preparing thereof |
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| CN102048791B (en) | 2012-05-23 |
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Address after: No. 19 Renmin South Road, Lingui District, Guilin City, Guangxi Zhuang Autonomous Region, 541100 Patentee after: GUILIN LAYN NATURAL INGREDIENTS Corp. Address before: 541100 Yangtang Industrial Park, Lingui Town, Lingui County, Guilin City, Guangxi Zhuang Autonomous Region Patentee before: GUILIN LAYN NATURAL INGREDIENTS Corp. |
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