CN105330711A - Extraction method for high-purity cornflower glucoside - Google Patents
Extraction method for high-purity cornflower glucoside Download PDFInfo
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- CN105330711A CN105330711A CN201510701510.6A CN201510701510A CN105330711A CN 105330711 A CN105330711 A CN 105330711A CN 201510701510 A CN201510701510 A CN 201510701510A CN 105330711 A CN105330711 A CN 105330711A
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Abstract
The invention relates to an extraction method for cornflower glucoside, and mainly relates to an extraction method for high-purity cornflower glucoside. The cornflower glucoside with the purity being more than 95% is extracted through the four steps of extraction, macroporous resin purification, first-time polyamide resin purification and second-time polyamide resin purification, and compared with the prior art, operation is easy, and the extraction purity is higher.
Description
Technical field
The present invention relates to a kind of extracting method of Minor centaury glycoside, relate generally to the highly purified extracting method of a kind of high purity Minor centaury glycoside.
Background technology
Anthocyanidin (Anthocyanidin), also known as cyanidin(e), is the water-soluble natural pigment that nature one class is extensively present in plant, belongs to flavonoids.Also be the main color-generation material in plant petals, the multicoloured color major parts such as fruit, vegetables, flowers are relevant with it.Anthocyanidin is present in the vacuole of vegetable cell, can be transformed by chlorophyll.Under the pH value condition that vegetable cell vacuole is different, petal is made to present multicoloured color.Autumn, soluble sugar increased, and cell is acid, takes on a red color in acid condition or purple, so petal is red, purple is anthocyanidin effect.
In view of the special role of anthocyanidin in food, health care, product category in the market about anthocyanidin is various, diversified in specifications, but be all the product that comparision contents is low mostly, in order to reduce dose, increase result of use, we developed the production method of high-content anthocyanidin Minor centaury glycoside.
Minor centaury glycoside, it is the main component in the anthocyanidin such as cowberry, black currant, blueberry, indigo fruit, black rice, Testa sojae atricolor, current method is that sour water or acid alcohol extract substantially, then by macroporous resin adsorption, obtains the Minor centaury glycoside of about 20%; Or again by additive method, the such as method such as gel, size-exclusion obtains the relatively high anthocyanidin of content.Relate to a kind of novel method of black rice anthocyanin extraction purification in 201210255787.7 patents, specifically comprise eight steps such as coarse reduction, fine grinding, water extraction, secondary water extraction, macroporous resin purification, nanofiltration, precooling, a lyophilize.The levigate defibrination of blend compounds body and the black rice flour of process of sieving adds water is pulverized by passing through, extracting at constant temperature, slurry slag separator carries out solid-liquid separation, be further purified by D101 type macroporous resin again, the ethanol elution of 55%-95% is first used again with distilled water, elutriant is the crude extract of anthocyanidin, crude extract is reclaimed ethanol by nanofiltration membrane (molecular weight is 100-200Da), finally carries out vacuum freezedrying and obtain black rice anthocyanin.The method process is loaded down with trivial details, high to equipment requirements, and needs the levigate defibrination of blend compounds body that added water by black rice flour, filtration difficulty.201410466396.9 relate to a kind of high purity black rice anthocyanin preparation technology in patent.The method is with common commercially available black rice for raw material, and its step comprises extraction, filtration, concentrated, purifying, desorbed solution are concentrated and dry, it is characterized in that adopting polyamide resin column purification, resolves with tartrate ethanol.The product look valency 500 that the method obtains, anthocyanidin content is about 50%.The method compares additive method, and product content is higher, but still improves a lot space.By above example, current method or be that content is lower, or be that process is loaded down with trivial details, equipment requirements strict, use filler expensive, production cost is high.
So we with cowberry, black currant, blueberry, indigo fruit, black rice, black soya bean for raw material, invented a kind of preparation method of high purity Minor centaury glycoside, the method can obtain the Minor centaury glycoside product of 20-95%.
Summary of the invention
The object of this invention is to provide a kind of simple to operate, the extracting method of the Minor centaury glycoside product that purity is higher.
The highly purified extracting method of a kind of high purity Minor centaury glycoside of the present invention, realizes as follows:
Step one, to extract: with cowberry, black currant, blueberry, indigo fruit, black rice, Testa sojae atricolor for raw material, with sulfuric acid water or the hydrochloric acid water of 3-10 times amount 0.1-0.5%, 30-50 DEG C to stir extraction 2 times each 2 hours, filters, merge filtered liquid;
Step 2, purification with macroreticular resin: by the absorption with macroporous adsorbent resin of step one gained filtrate by handling well, loading flow velocity 2-5BV/h, the pure washing of 3-5BV is mixed to pH5-6,3-5BV70-85% alcohol is resolved, flow velocity 1-1.5BV/h, desorbed solution is concentrated into proportion 1.03-1.1, spraying dry, obtain powder-product, this product Minor centaury glycoside content 20-30%;
Step 3, for the first time polyamide resin purifying: by step 2 products obtained therefrom, add 1-3 times of pure water, stir, adsorbed by the polyamide resin handled well, pure washing is assorted, 60-70% alcohol is resolved, is concentrated into without alcohol, spraying dry, obtain powder-product, this product Minor centaury glycoside content 60-75%;
Step 4, second time polyamide resin purifying: the product of gained in step 3 is added the polymeric amide handled well in right amount, dry, then load in processed good polyamide resin column, with sherwood oil: ethyl acetate: phosphoric acid (300-100): (100-200): 0.5 as elutriant, Fractional Collections, TLC detects, component containing Minor centaury glycoside is merged, concentrate drying, obtains powder-product, and this product Minor centaury glycoside content is greater than 95%.
Embodiment
Technical solution of the present invention is not limited to cited embodiment, also comprises any combination in embodiment.
Embodiment one, the highly purified extracting method of a kind of high purity Minor centaury glycoside of the present invention, realize as follows:
Step one, to extract: with cowberry, black currant, blueberry, indigo fruit, black rice, Testa sojae atricolor for raw material, with the sulfuric acid water of 3 times amount 0.1%, 30 DEG C to stir extraction 2 times each 2 hours, filters, merging filtered liquid;
Step 2, purification with macroreticular resin: by the absorption with macroporous adsorbent resin of step one gained filtrate by handling well, loading flow velocity 2BV/h, the pure washing of 3BV is mixed to pH5,3BV70% alcohol is resolved, flow velocity 1BV/h, desorbed solution is concentrated into proportion 1.03, spraying dry, obtain powder-product, this product Minor centaury glycoside content 20-30%;
Step 3, for the first time polyamide resin purifying: by step 2 products obtained therefrom, add 1 times of pure water, stir, adsorbed by the polyamide resin handled well, pure washing is assorted, 60% alcohol is resolved, is concentrated into without alcohol, spraying dry, obtain powder-product, this product Minor centaury glycoside content 60-75%;
Step 4, second time polyamide resin purifying: the product of gained in step 3 is added the polymeric amide handled well in right amount, dry, then load in processed good polyamide resin column, with sherwood oil: ethyl acetate: phosphoric acid 300:100:0.5 as elutriant, Fractional Collections, TLC detects, component containing Minor centaury glycoside is merged, concentrate drying, obtains powder-product, and this product Minor centaury glycoside content is greater than 95%.
Embodiment two, the highly purified extracting method of a kind of high purity Minor centaury glycoside of the present invention, realize as follows:
Step one, to extract: with cowberry, black currant, blueberry, indigo fruit, black rice, Testa sojae atricolor for raw material, with the hydrochloric acid water of 5 times amount 0.2%, 40 DEG C to stir extraction 2 times each 2 hours, filters, merging filtered liquid;
Step 2, purification with macroreticular resin: by the absorption with macroporous adsorbent resin of step one gained filtrate by handling well, loading flow velocity 3BV/h, the pure washing of 4BV is mixed to pH5.2,4BV73% alcohol is resolved, flow velocity 1.2BV/h, desorbed solution is concentrated into proportion 1.05, spraying dry, obtain powder-product, this product Minor centaury glycoside content 20-30%;
Step 3, for the first time polyamide resin purifying: by step 2 products obtained therefrom, add 2 times of pure water, stir, adsorbed by the polyamide resin handled well, pure washing is assorted, 63% alcohol is resolved, is concentrated into without alcohol, spraying dry, obtain powder-product, this product Minor centaury glycoside content 60-75%;
Step 4, second time polyamide resin purifying: the product of gained in step 3 is added the polymeric amide handled well in right amount, dry, then load in processed good polyamide resin column, with sherwood oil: ethyl acetate: phosphoric acid 250:120:0.5 as elutriant, Fractional Collections, TLC detects, component containing Minor centaury glycoside is merged, concentrate drying, obtains powder-product, and this product Minor centaury glycoside content is greater than 95%.
Embodiment three, the highly purified extracting method of a kind of high purity Minor centaury glycoside of the present invention, realize as follows:
Step one, to extract: with cowberry, black currant, blueberry, indigo fruit, black rice, Testa sojae atricolor for raw material, with 7 times amount 0.3% hydrochloric acid waters, 35 DEG C to stir extraction 2 times each 2 hours, filters, merging filtered liquid;
Step 2, purification with macroreticular resin: by the absorption with macroporous adsorbent resin of step one gained filtrate by handling well, loading flow velocity 4BV/h, the pure washing of 5BV is mixed to pH5.4,5BV75% alcohol is resolved, flow velocity 1.3BV/h, desorbed solution is concentrated into proportion 1.07, spraying dry, obtain powder-product, this product Minor centaury glycoside content 20-30%;
Step 3, for the first time polyamide resin purifying: by step 2 products obtained therefrom, add 3 times of pure water, stir, adsorbed by the polyamide resin handled well, pure washing is assorted, 65% alcohol is resolved, is concentrated into without alcohol, spraying dry, obtain powder-product, this product Minor centaury glycoside content 60-75%;
Step 4, second time polyamide resin purifying: the product of gained in step 3 is added the polymeric amide handled well in right amount, dry, then load in processed good polyamide resin column, with sherwood oil: ethyl acetate: phosphoric acid 200:140:0.5 as elutriant, Fractional Collections, TLC detects, component containing Minor centaury glycoside is merged, concentrate drying, obtains powder-product, and this product Minor centaury glycoside content is greater than 95%.
Embodiment four, the highly purified extracting method of a kind of high purity Minor centaury glycoside of the present invention, realize as follows:
Step one, to extract: with cowberry, black currant, blueberry, indigo fruit, black rice, Testa sojae atricolor for raw material, with the sulfuric acid water of 9 times amount 0.5%, 45 DEG C to stir extraction 2 times each 2 hours, filters, merging filtered liquid;
Step 2, purification with macroreticular resin: by the absorption with macroporous adsorbent resin of step one gained filtrate by handling well, loading flow velocity 5BV/h, the pure washing of 5BV is mixed to pH5.8,5BV80% alcohol is resolved, flow velocity 1.4BV/h, desorbed solution is concentrated into proportion 1.08, spraying dry, obtain powder-product, this product Minor centaury glycoside content 20-30%;
Step 3, for the first time polyamide resin purifying: by step 2 products obtained therefrom, add 3 times of pure water, stir, adsorbed by the polyamide resin handled well, pure washing is assorted, 68% alcohol is resolved, is concentrated into without alcohol, spraying dry, obtain powder-product, this product Minor centaury glycoside content 60-75%;
Step 4, second time polyamide resin purifying: the product of gained in step 3 is added the polymeric amide handled well in right amount, dry, then load in processed good polyamide resin column, with sherwood oil: ethyl acetate: phosphatase 11 50:160:0.5 as elutriant, Fractional Collections, TLC detects, component containing Minor centaury glycoside is merged, concentrate drying, obtains powder-product, and this product Minor centaury glycoside content is greater than 95%.
Embodiment five, the highly purified extracting method of a kind of high purity Minor centaury glycoside of the present invention, realize as follows:
Step one, to extract: with cowberry, black currant, blueberry, indigo fruit, black rice, Testa sojae atricolor for raw material, with the sulfuric acid water of 10 times amount 0.5%, 50 DEG C to stir extraction 2 times each 2 hours, filters, merging filtered liquid;
Step 2, purification with macroreticular resin: by the absorption with macroporous adsorbent resin of step one gained filtrate by handling well, loading flow velocity 2BV/h, the pure washing of 3BV is mixed to pH6,3BV85% alcohol is resolved, flow velocity 1.5BV/h, desorbed solution is concentrated into proportion 1.1, spraying dry, obtain powder-product, this product Minor centaury glycoside content 20-30%;
Step 3, for the first time polyamide resin purifying: by step 2 products obtained therefrom, add 1.5 times of pure water, stir, adsorbed by the polyamide resin handled well, pure washing is assorted, 70% alcohol is resolved, is concentrated into without alcohol, spraying dry, obtain powder-product, this product Minor centaury glycoside content 60-75%;
Step 4, second time polyamide resin purifying: the product of gained in step 3 is added the polymeric amide handled well in right amount, dry, then load in processed good polyamide resin column, with sherwood oil: ethyl acetate: phosphatase 11 00:200:0.5 as elutriant, Fractional Collections, TLC detects, component containing Minor centaury glycoside is merged, concentrate drying, obtains powder-product, and this product Minor centaury glycoside content is greater than 95%.
The present invention illustrate and describes embodiments of the invention, the those of ordinary skill of the invention of this area is appreciated that, can carry out multiple change, amendment and replacement to these embodiments when not departing from principle of the present invention and aim, scope of the present invention is by claim extremely equivalents.
Claims (1)
1. an extracting method for high purity Minor centaury glycoside, is characterized in that: described extracting method comprises
Step one, to extract: with cowberry, black currant, blueberry, indigo fruit, black rice, Testa sojae atricolor for raw material, with sulfuric acid water or the hydrochloric acid water of 3-10 times amount 0.1-0.5%, 30-50 DEG C to stir extraction 2 times each 2 hours, filters, merge filtered liquid;
Step 2, purification with macroreticular resin: by the absorption with macroporous adsorbent resin of step one gained filtrate by handling well, loading flow velocity 2-5BV/h, the pure washing of 3-5BV is mixed to pH5-6,3-5BV70-85% alcohol is resolved, flow velocity 1-1.5BV/h, desorbed solution is concentrated into proportion 1.03-1.1, spraying dry, obtain powder-product, this product Minor centaury glycoside content 20-30%;
Step 3, for the first time polyamide resin purifying: by step 2 products obtained therefrom, add 1-3 times of pure water, stir, adsorbed by the polyamide resin handled well, pure washing is assorted, 60-70% alcohol is resolved, is concentrated into without alcohol, spraying dry, obtain powder-product, this product Minor centaury glycoside content 60-75%;
Step 4, second time polyamide resin purifying: the product of gained in step 3 is added the polymeric amide handled well in right amount, dry, then load in processed good polyamide resin column, with sherwood oil: ethyl acetate: phosphoric acid (300-100): (100-200): 0.5 as elutriant, Fractional Collections, TLC detects, component containing Minor centaury glycoside is merged, concentrate drying, obtains powder-product, and this product Minor centaury glycoside content is greater than 95%.
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Application publication date: 20160217 |