CN102675139A - Method for extracting ceramide from konjak flying powder - Google Patents
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Abstract
A method for extracting ceramide from konjak flying powder is composed of eight procedures of material sorting, comprehensive extracting, concentrating, extracting, gradient eluting, drying, secondary gradient eluting and drying. The method has the advantages that by conducting ultrasonic extracting under the conditions of appropriate ethanol concentration, solid-liquid ration, temperature and soaking method and time, amount of a ceramide component leaking from the konjak flying powder can be increased, and extraction rate is improved; and the purity of the ceramide can be improved through multi-extraction and the gradient eluting by using appropriate solvent combination and proportions of the combination. The extraction rate of the ceramide from the konjak flying powder is 75%, and the purity of the ceramide is 95.5%.
Description
Technical field
The present invention relates to from konjaku, extract the method for active substance, particularly a kind of method of from fry starch of konjak, extracting ceramide.
Background technology
Konjaku is useful basic food, and to the too much people of edible animal property acidic food, konjaku is eaten in collocation, can reach food acids, soda balance, and is favourable to HUMAN HEALTH; At present health care, the medical functions of konjaku many clinical experimental studies have been made all over the world; The conclusion basically identical; Wherein the staple Rhizoma amorphophalli glucomannan belongs to water-soluble hemicellulose, and its outstanding nutrient health-care function is to bring into play the regulating effect of food fibre to nutritional imbalance, contained non-water-soluble fiber in the greengroceries such as it and Chinese cabbage, celery; Original shape discharge person is different after getting into human body, and it can participate in the metabolism of human body and influence entero-bacte changing to helping healthy direction; Konjaku is except that containing a large amount of konjac glucomannas; The amino acid and 10 kinds of mineral trace elements and the abundant foodstuff fibre that also contain vegeto-alkali, pectin, 17 kinds of needed by human body; It is the unique plant that contains a large amount of konjac glucomannas of organic sphere; Modern rich man diseases such as hyperlipidemia, hypercholesterolemia, mellitus, obesity, constipation are had good preventive and therapeutic effect, are middle-aged and old ideal heath food, receive the favor of world's health food market deeply; In Japan, konjaku becomes the indispensable delicacies of seat seat already, is described as " magic power food ".
Rhizoma amorphophalli glucomannan also has performances such as thickening, emulsification, gelling, bonding, water conservation; Its powder promptly can be used as major ingredient and makes various food; Also can be used as foodstuff additive to improve the quality of other food; In foodstuffs industry, be used as foodstuff additive such as thickening material, suspended emulsion agent, emulsifying agent, stablizer, quality improver, be widely used in cereal product, meat product, beverage, seasonings, the bean product; Also can be used for fields such as makeup, textile industry, construction industry, consumable film, environment protection, historical relic's protection in addition.
Owing to the extensive use of konjaku and all over the world to the understanding of konjaku, make that the market requirement of konjaku is increasing, formed three big markets such as Japanese market, Korea S and market, South East Asia, American-European market at present.Needed both at home and abroad 900,000 tons of fresh Amorphophallus rivieris in 2006, and only 520,000 tons of output can't be satisfied the demand far away.Since the eighties in 20th century, Chinese konjaku has begun industrialized development, and cultivated area and processing amount are all in develop rapidly; At produced simultaneously a large amount of fry starch of konjak of producing, because the anti-nutrition of fry starch of konjak and contain peculiar smell is generally all passed into disuse; Not only waste, and contaminate environment.But the content of ceramide reaches 0.15%-0.20% in the fry starch of konjak, compares with other sources such as soybean, wheats, and content is higher relatively.Ceramide is an important function material in the organism, has antitumor, anti-hepatovirus, reducing blood-fat, hypoglycemic, fat-reducing, anti-ageing, effect such as whiten, and is widely used in the Medicines and Health Product, is of very high actual application value.So from fry starch of konjak, extract ceramide is an approach that well increases economic benefit and social benefit.
In the prior art; The method that a lot of extraction konjak ceramides are arranged; Number of patent application 2011103279658 has been announced " a kind of method that from fry starch of konjak, prepares ceramide "; This method with alcohol immersion extraction, petroleum ether extraction, with petroleum ether-ethyl acetate through the silicagel column gradient elution, then with alcohol-water through C18 bonded silica gel ODS post gradient elution, obtain ceramide content at last and reach the sample more than 95%, though this method is fine; But because initial process for extracting problem makes extraction yield not high; Number of patent application 2010105989816 has been announced " konjak ceramide is process for extracting extremely "; This method adopts the ethanol extracted many times; Concentrate with ethyl acetate extraction then; Dissolve repeatedly, extract, concentrate with ethanol, ETHYLE ACETATE and sherwood oil again, the ceramide product content that obtains at last is too low.
Summary of the invention
Technical problem to be solved by this invention is the deficiency to prior art; A kind of combined extraction method is provided; Raising is adopted suitable solvent combination and ratio thereof to carry out gradient elution through silicagel column then and is extracted highly purified ceramide product the extraction yield of ceramide; To increase economic efficiency.
For solving the problems of the technologies described above; The technical scheme that the present invention adopted is a kind of method of from fry starch of konjak, extracting ceramide; By select materials, comprehensively extract, concentrate, extraction, gradient elution, drying, gradient elution and dry eight big operations completion once more, concrete grammar is following.
⑴ select materials: collect fry starch of konjak, remove impurity.
⑵ comprehensively extract: fry starch of konjak is used 70% ethanolic soln under 70 ℃ of temperature, stir as the standard of 1:5-6 according to solid-to-liquid ratio and soak 10-20min; Use the ultrasonic extraction 40min of 600W power again; And then stir and soak 10-20min, it is centrifugal then will to extract leach liquor, gets supernatant; And then filter residue used 95% ethanolic soln soak under 70 ℃ of temperature as the standard of 1:4-5 according to solid-to-liquid ratio; With the ultrasonic extraction 30min of 600W power, and then stir and soak 10-20min, it is centrifugal then will to extract leach liquor; Get supernatant, at last twice supernatant merged.
⑷ extraction: liquid concentrator is stirred extraction 40-50min with the sherwood oil of 3-5 times of volume under 60 ℃ of temperature, standing demix 30min then, collection sherwood oil phase; And then repeat twice; Merge the sherwood oil phase, concentrate, obtain ceramide medicinal extract.
⑸ gradient elution: with silica gel wet method dress post and with after the eluent balance; With appearance on the ceramide medicinal extract; Adopt petroleum ether-ethyl acetate dissolution with solvents and gradient elution; The graded order of elutriant is a sherwood oil: ETHYLE ACETATE=19:1 to 1:19 volume ratio, substep is collected effluent, merges the effluent with identical component.
⑹ dry: distillating recovering solvent, and leave standstill residue and separate out white floss, centrifugal collection after drying gets the ceramide bullion.
⑺ once more gradient elution: with silica gel wet method dress post and with after the eluent balance; The ceramide bullion is gone up appearance with eluent dissolving back; Adopting alcohol-water is dissolution with solvents and gradient elution; The graded order of eluent is an ethanol: water=19:1 to 1:1 volume ratio, substep is collected effluent, merges the effluent with identical component.
⑻ dry: distillating recovering solvent, and to leave standstill residue and separate out white floss, the lyophilize of centrifugal collection final vacuum gets the ceramide powder; Detect through HPLC-ELSD, the content of ceramide reaches 95.5% in the powder.
The invention has the beneficial effects as follows: adopt suitable alcohol concn, solid-to-liquid ratio, temperature, immersion process and time and ultrasonic extraction, can improve the component that the ceramide composition infiltrates from fry starch of konjak, improve extraction yield; Through repeatedly extracting and adopt suitable solvent combination and ratio thereof to carry out gradient elution through silicagel column, can improve the purity of ceramide again, the present invention extracts the extraction rate reached 75% of ceramide from fry starch of konjak, and purity reaches 95.5%.
Embodiment
Below in conjunction with embodiment the present invention is described further.
Embodiment 1.
Get fry starch of konjak 1kg, the ethanolic soln 5kg with 70% stirs under 70 ℃ of temperature and soaks 10min, uses the ultrasonic extraction 40min of 600W power again, and then stirs and soak 10min, and it is centrifugal to extract leach liquor then, gets supernatant; And then filter residue soaked under 70 ℃ of temperature with 95% ethanolic soln 4kg, with the ultrasonic extraction 30min of 600W power, and then stir and soak 10min, it is centrifugal to extract leach liquor, gets supernatant, at last with twice supernatant merging; Ethanol is reclaimed in redistillation, debris is concentrated with Rotary Evaporators obtain sticky shape material 50.5g; Under 60 ℃ of temperature, stir extraction 40min with 100 milliliters of sherwood oils then, standing demix 30min collects the sherwood oil phase then; And then repeat twice; Merge the sherwood oil phase, concentrate, obtain ceramide medicinal extract 23.7g; With silica gel wet method dress post and with petroleum ether-ethyl acetate eluent balance, ceramide medicinal extract is gone up appearance with the petroleum ether-ethyl acetate dissolving, adopt petroleum ether-ethyl acetate to dissolve gradient elution; The graded order is a sherwood oil: ETHYLE ACETATE=19:1 to 1:19 volume ratio; Substep is collected effluent, merges the effluent with identical component, then distillating recovering solvent; Leave standstill residue and separate out white floss, centrifugal collection after drying gets ceramide bullion 7.12g; Gradient elution once more: with silica gel wet method dress post and with after the alcohol-water eluent balance, the ceramide bullion is gone up kind with alcohol-water eluent dissolving back, the employing alcohol-water is the eluent gradient elution; The graded order of eluent is an ethanol: water=19:1 to 1:1 volume ratio; Substep is collected effluent, merges the effluent with identical component, then distillating recovering solvent; Leave standstill residue and separate out white floss, the lyophilize of centrifugal collection final vacuum gets ceramide powder 1.21g; Detect through HPLC-ELSD, the content of ceramide is 95.5% in the powder, and the former content that flies ceramide in the powder is 0.152%, and extraction yield is 76.02%.
Embodiment 2.
Get fry starch of konjak 100kg, the ethanolic soln 600kg with 70% stirs under 70 ℃ of temperature and soaks 15min, uses the ultrasonic extraction 40min of 600W power again, and then stirs and soak 15min, and it is centrifugal to extract leach liquor then, gets supernatant; And then filter residue soaked under 70 ℃ of temperature with 95% ethanolic soln 500kg, with the ultrasonic extraction 30min of 600W power, and then stir and soak 15min, it is centrifugal to extract leach liquor, gets supernatant, at last with twice supernatant merging; Ethanol is reclaimed in redistillation, debris is concentrated with Rotary Evaporators obtain sticky shape material 4.97kg; Under 60 ℃ of temperature, stir extraction 45min with 10 liters of sherwood oils then, standing demix 30min collects the sherwood oil phase then; And then repeat twice; Merge the sherwood oil phase, concentrate, obtain ceramide medicinal extract 2.25kg; With silica gel wet method dress post and with petroleum ether-ethyl acetate eluent balance, ceramide medicinal extract is gone up appearance with the petroleum ether-ethyl acetate dissolving, adopt petroleum ether-ethyl acetate to dissolve gradient elution; The graded order is a sherwood oil: ETHYLE ACETATE=19:1 to 1:19 volume ratio; Substep is collected effluent, merges the effluent with identical component, then distillating recovering solvent; Leave standstill residue and separate out white floss, centrifugal collection after drying gets ceramide bullion 657g; Gradient elution once more: with silica gel wet method dress post and with after the alcohol-water eluent balance, the ceramide bullion is gone up kind with alcohol-water eluent dissolving back, the employing alcohol-water is the eluent gradient elution; The graded order of eluent is an ethanol: water=19:1 to 1:1 volume ratio; Substep is collected effluent, merges the effluent with identical component, then distillating recovering solvent; Leave standstill residue and separate out white floss, the lyophilize of centrifugal collection final vacuum gets ceramide powder 118g; Detect through HPLC-ELSD, the content of ceramide is 95.1% in the powder, and the former content that flies ceramide in the powder is 0.152%, and extraction yield is 73.82%.
Embodiment 3.
Get fry starch of konjak 1000kg, the ethanolic soln 5500kg with 70% stirs under 70 ℃ of temperature and soaks 20min, uses the ultrasonic extraction 40min of 600W power again, and then stirs and soak 20min, and it is centrifugal to extract leach liquor then, gets supernatant; And then filter residue soaked under 70 ℃ of temperature with 95% ethanolic soln 4500kg, with the ultrasonic extraction 30min of 600W power, and then stir and soak 20min, it is centrifugal to extract leach liquor, gets supernatant, at last with twice supernatant merging; Ethanol is reclaimed in redistillation, debris is concentrated with Rotary Evaporators obtain sticky shape material 48.9kg; Under 60 ℃ of temperature, stir extraction 50min with 100 liters of sherwood oils then, standing demix 30min collects the sherwood oil phase then; And then repeat twice; Merge the sherwood oil phase, concentrate, obtain ceramide medicinal extract 22.2kg; With silica gel wet method dress post and with petroleum ether-ethyl acetate eluent balance, ceramide medicinal extract is gone up appearance with the petroleum ether-ethyl acetate dissolving, adopt petroleum ether-ethyl acetate to dissolve gradient elution; The graded order is a sherwood oil: ETHYLE ACETATE=19:1 to 1:19 volume ratio; Substep is collected effluent, merges the effluent with identical component, then distillating recovering solvent; Leave standstill residue and separate out white floss, centrifugal collection after drying gets ceramide bullion 6.37kg; Gradient elution once more: with silica gel wet method dress post and with after the alcohol-water eluent balance, the ceramide bullion is gone up kind with alcohol-water eluent dissolving back, the employing alcohol-water is the eluent gradient elution; The graded order of eluent is an ethanol: water=19:1 to 1:1 volume ratio; Substep is collected effluent, merges the effluent with identical component, then distillating recovering solvent; Leave standstill residue and separate out white floss, the lyophilize of centrifugal collection final vacuum gets ceramide powder 1151g; Detect through HPLC-ELSD, the content of ceramide is 94.8% in the powder, and the former content that flies ceramide in the powder is 0.152%, and extraction yield is 71.79%.
Claims (1)
1. from fry starch of konjak, extract the method for ceramide, by select materials, comprehensively extract, concentrate, extraction, gradient elution, drying, gradient elution and dry eight big operations completion once more, it is characterized in that concrete grammar is following:
⑴ select materials: collect fry starch of konjak, remove impurity;
⑵ comprehensively extract: fry starch of konjak is used 70% ethanolic soln under 70 ℃ of temperature, stir as the standard of 1:5-6 according to solid-to-liquid ratio and soak 10-20min; Use the ultrasonic extraction 40min of 600W power again; And then stir and soak 10-20min, it is centrifugal then will to extract leach liquor, gets supernatant; And then filter residue used 95% ethanolic soln soak under 70 ℃ of temperature as the standard of 1:4-5 according to solid-to-liquid ratio; With the ultrasonic extraction 30min of 600W power, and then stir and soak 10-20min, it is centrifugal then will to extract leach liquor; Get supernatant, at last twice supernatant merged;
⑷ extraction: liquid concentrator is stirred extraction 40-50min with the sherwood oil of 3-5 times of volume under 60 ℃ of temperature, standing demix 30min then, collection sherwood oil phase; And then repeat twice; Merge the sherwood oil phase, concentrate, obtain ceramide medicinal extract;
⑸ gradient elution: with silica gel wet method dress post and with after the eluent balance; With appearance on the ceramide medicinal extract; Adopt petroleum ether-ethyl acetate dissolution with solvents and gradient elution; The graded order of elutriant is a sherwood oil: ETHYLE ACETATE=19:1 to 1:19 volume ratio, and substep is collected effluent, merges the effluent with identical component;
⑹ dry: distillating recovering solvent, and leave standstill residue and separate out white floss, centrifugal collection after drying gets the ceramide bullion;
⑺ once more gradient elution: with silica gel wet method dress post and with after the eluent balance; The ceramide bullion is gone up appearance with eluent dissolving back; Adopting alcohol-water is dissolution with solvents and gradient elution; The graded order of eluent is an ethanol: water=19:1 to 1:1 volume ratio, and substep is collected effluent, merges the effluent with identical component;
⑻ dry: distillating recovering solvent, and to leave standstill residue and separate out white floss, the lyophilize of centrifugal collection final vacuum gets the ceramide powder.
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| CN103755583A (en) * | 2014-01-27 | 2014-04-30 | 广州市娇兰化妆品有限公司 | Method for extracting and separating ceramide in konjac flying powder |
| CN106008253A (en) * | 2016-05-25 | 2016-10-12 | 湖南华诚生物资源股份有限公司 | Method for extracting high-purity ceramide from rice bran |
| CN108623492A (en) * | 2017-03-18 | 2018-10-09 | 成都希福生物科技有限公司 | A method of the high efficiency extraction ceramide from konjaku |
| CN108947864A (en) * | 2018-06-08 | 2018-12-07 | 三原利华生物技术有限公司 | A kind of preparation method of ceramide |
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| CN113416184A (en) * | 2021-07-22 | 2021-09-21 | 南京师范大学 | Method for extracting isoschaftoside, vitexin and alkaloid from konjak |
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- 2012-05-03 CN CN2012101332077A patent/CN102675139A/en active Pending
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| CN103082169B (en) * | 2013-02-08 | 2014-12-31 | 中美御康生物科技（北京）有限公司 | Composite collagenous fruit powder |
| CN103755583A (en) * | 2014-01-27 | 2014-04-30 | 广州市娇兰化妆品有限公司 | Method for extracting and separating ceramide in konjac flying powder |
| CN103755583B (en) * | 2014-01-27 | 2015-07-01 | 广州市娇兰化妆品有限公司 | Method for extracting and separating ceramide in konjac flying powder |
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| CN108623492A (en) * | 2017-03-18 | 2018-10-09 | 成都希福生物科技有限公司 | A method of the high efficiency extraction ceramide from konjaku |
| CN108947864A (en) * | 2018-06-08 | 2018-12-07 | 三原利华生物技术有限公司 | A kind of preparation method of ceramide |
| CN109265501A (en) * | 2018-11-15 | 2019-01-25 | 派能生物科技（深圳）有限公司 | A kind of method and application for extracting ceramide from pineapple |
| CN110438177A (en) * | 2019-08-12 | 2019-11-12 | 三原利华生物技术有限公司 | A method of ceramide is prepared from apple juicing pomace |
| CN111499537A (en) * | 2020-05-12 | 2020-08-07 | 深圳市三也生物科技有限公司 | Refining and purifying method of plant-derived ceramide extract |
| CN113416184A (en) * | 2021-07-22 | 2021-09-21 | 南京师范大学 | Method for extracting isoschaftoside, vitexin and alkaloid from konjak |
| CN113416184B (en) * | 2021-07-22 | 2023-09-22 | 南京师范大学 | Method for extracting isosaftoside, vitexin and alkaloid from konjak |
| CN113788864A (en) * | 2021-10-23 | 2021-12-14 | 绵阳膳意生物科技有限公司 | Co-production preparation method of ceramide and glucoside (lipid) acyl sphingosine |
| JP7273427B1 (en) | 2021-12-24 | 2023-05-15 | 雪国アグリ株式会社 | Water-soluble konjac potato extract and method for producing the same |
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Application publication date: 20120919 |