CN1237896C - Method for producing base material of soybean isoflavone with sugariness taste - Google Patents
Method for producing base material of soybean isoflavone with sugariness taste Download PDFInfo
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- CN1237896C CN1237896C CNB031398952A CN03139895A CN1237896C CN 1237896 C CN1237896 C CN 1237896C CN B031398952 A CNB031398952 A CN B031398952A CN 03139895 A CN03139895 A CN 03139895A CN 1237896 C CN1237896 C CN 1237896C
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- isoflavones
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Abstract
Te the present invention relates to a method for producing base material of sweet soybean isoflavone, which comprises a raw ma pretreatment of soybean embryos, etc. and extracting, purifying and preparation methods of soybean isoflavone. Firstly, after the raw material (mainly comprising the soybean embryos) richly containing the soybean isoflavone is preprocessed by certain heat, water is added to the raw material, and the raw material is extracted under certain temperature. After primary centrifugation is carried out, filtered liquor richly containing the isoflavone can be obtained by filtration. Moreover, macro-porous adsorption resin is used for adsorbing isoflavone compounds in the filtered liquor. Subsequently, ethanol (whose concentration in volume percent is 40 to 70%) is used for elution. After alcohol is removed from obtained eluant, obtained extracted liquor is the liquid base material richly containing the sweet soybean isoflavone. The liquid base material can be further made into quick-dissolving isoflavone powdery base material with good flavor by spray-drying or freeze-drying. The base material of the soybean isoflavone, which is produced by the method, can be used for common food and healthcare food (particularly for oral medicinal liquid).
Description
Technical field
The present invention relates to the technical field of producing of isoflavones, specifically be meant a kind of production method of sweet flavor isoflavones base-material.
Background technology
Isoflavones is one of main functional components of soybean, studies show that in a large number it has physiological functions such as significant anti-cancer activity, prevention of osteoporosis disease effect and angiocardiopathy effect, has become the focus of people's research and development at present.Usually, the isoflavone content in the soybean germ (or plumular axis) is far above the cotyledon position, and the former is about 30～60 times of the latter.On the other hand, produce a large amount of plumule accessory substances in the production process of soybean protein, thereby soybean germ is the optimum feed stock of producing the isoflavones product.
The isoflavone compounds that exists in the soybean has three major types; 12 kinds of compounds altogether; be respectively acidylate (acetylation and malonylization etc.) glucoside, glucoside (daidzin (Daidzin), genistin (Genistin) and daidzin (Glycitin)), and three types of aglucons (comprising daidzein (Daidzein), genistein (Genistein) and Daidezin (Glycitein)).The existence form of isoflavones in soybean is mainly with malonyl glucosides form and exists, and glucosides and aglucon shape are seldom.The general less stable of malonyl glucosides becomes the acetylated glucoside form easily when soybean processing, even the glucosides form.For example, it is heated and can sloughs a CO
2Become the acetyl glucosides.In general, malonyl type isoflavone glucoside (the main natural existence form of isoflavones) often presents hardship, astringent taste, the key constraints that is considered to soybean, however their glucosides type compound is certain sweet local flavor, and the bitter taste of aglucon type compound is stronger.As seen, the main existence form of isoflavones in the soybean is converted to the glucosides type, is extremely important for their further development and use by certain preliminary treatment.
Home and abroad big quantity research (being mainly experiment in vitro) shows that aglucon type isoflavones has the strongest antioxidation activity, perhaps other related activity.Therefore, the relevant patent of the production of a large amount of isoflavones that the home and abroad occurs or preparation all is to be main target with aglucon type isoflavones.Yet aglucon type isoflavones has very strong bitter taste, thereby causes the isoflavones product of home and abroad mainly to occur with tablet or capsule product form.Because the bad flavor of aglucon type isoflavones has limited it as other food form, or the application in normal food.In fact, the biologically active of relevant isoflavones in human body is then unlike research that in vitro study drew, there are several to studies show that the isoflavone glucoside compound has the biologically active the same with the aglucon type in giving birth to body recently, because have alpha-glucosidase and β--the glycosidase of q.s in the digestive system of human body, make the glucosides type isoflavones of ingesting be converted to the aglucon type.In addition, also have one and studies confirm that some glucoside type flavone compound can directly be absorbed by human body, the rate of decay of glucosides type compound in blood of human body is starkly lower than aglucon type compound, that is to say that its drug effect is more lasting.
In addition, the production of present isoflavones or preparation technology mostly adopt organic solvent as extractant.The major defect of this extracting method is to have increased production cost, and is unfavorable for the production of food-grade base-material.
Summary of the invention
Purpose of the present invention is exactly in order to solve above-mentioned the deficiencies in the prior art part, and a kind of production method of sweet flavor isoflavones base-material is provided.This method can obtain having special solely local flavor and water-soluble good isoflavones base-material, and this base-material can be widely used in the middle of normal food, the functional or health food, more particularly at functional or health foods such as women's oral liquid, beverages.
The production method of a kind of sweet flavor isoflavones base-material of the present invention is characterized in that it comprises the steps and process conditions:
The first step with the soybean germ raw material of drying 120～180 ℃ of following heat treated 15～60 minutes;
Second step is in soybean germ, according to kilogram: the solid-to-liquid ratios of total extractant (raw material with) adds water to rise solid-to-liquid ratio 1: 8～15, in the extraction 0.5 hour～3 hours down of 80 ℃～little fluidized state, filtration;
The 3rd step filtrate is left standstill after 6～24 hours under 4～25 ℃ centrifugal through clarification or filtration treatment;
Supernatant after the 4th step is centrifugal adopts hyperfiltration treatment, and the ultrafiltrate vacuum concentrates and gets final product.
In order to realize the present invention better, heating condition the best of the described first step is 160～180 ℃ of following heat treated 20～45 minutes; The optimum extraction condition in described second step is 90～95 ℃ and extracted 1～2 hour down that extractant is a water, filtered through gauze, merging filtrate behind the triplicate; The molecule interception of the milipore filter in described the 4th step hyperfiltration treatment is between 10,000～30,000; The supernatant in described the 4th step enters the macroporous absorbent resin post and adsorbs, flow velocity is (3～5) BV/ hour, adopt the individual BV of deionized water rinsing (3～4) then, then carry out wash-out, eluant, eluent employing percent by volume is 40～70% ethanolic solution, gained isoflavones eluent vacuum concentrates goes alcohol to get final product, and this can reduce the production cost of isoflavones to a certain extent; Described macroporous absorbent resin is NAK-8, NAK-12 or X-5; Described the 4th isoflavones base-material that obtains of step is isoflavones liquid-type base-material or paste liquid base material, and also further spray-drying makes powdered isoflavones base-material.
Be applicable to that raw material of the present invention mainly is a soybean germ, the quality of raw material itself and isoflavone content have certain influence to the quality and the yield of finished product.Key of the present invention is the preliminary treatment (being heat treated) to soybean germ, and suitably the heat pre-treatment of degree has material impact to the quality of entire product, because it influences the existence form of isoflavones in the soybean germ.Soybean germ through pre-place product does not need to do further pulverizing, adopts full plumule to extract, and helps follow-up filtration.When adopting water to extract, can consider under little fluidized state, to extract, can extract the isoflavone compounds in the plumule effectively, shorten extraction time.In general, little fluidized state extracted 30～60 minutes down, three times altogether, can extract most of water miscible isoflavone compounds in the plumule very effectively.
But the sweetness of both production low-purity of the present invention flavor isoflavones base-material (paste or Powdered) also can be produced the goods (liquid or Powdered) of higher degree.During the isoflavones goods of production low-purity, the operation of having adopted milipore filter to separate mainly is in order to remove some soluble macromolecule or colloids in the extract, thereby has avoided concentration process to bubble and problems such as flocculation.As for producing highly purified isoflavones goods, the present invention mainly adopts macroreticular resin absorption purifying, in order to obtain the more mellow isoflavones of sweet flavor, can collected volume percentage is the elution fraction (specifically deciding according to product) of 20～50% ethanolic solution.
The present invention compared with prior art has following advantage and beneficial effect:
1. the present invention is with a kind of special technology, produce isoflavones goods with unique sweet flavor, color and luster is bright, water-soluble splendid, there is pained deficiency thereby solved existing isoflavones product, thereby is with a wide range of applications at food such as oral liquid, beverage and buccal tablet or health food.
2. the present invention adopts water as extractant, has avoided the employing organic solvent, thereby has simplified production technology and cost, and more helps the application prospect at food.
3. but the isoflavones base-material of both production low-purity of the present invention also can be produced highly purified isoflavones base-material (deciding according to concrete purposes), and production cost is low, added value is high.
4. the quality of the isoflavones product of the present invention's production can meet or exceed international like product, and purposes is more extensive.Producing raw materials used is the accessory substance of soybean processing, has both improved the added value of agricultural byproducts, has very high social benefit and economic benefit, will fill up the blank of domestic sweet flavor type isoflavones product again.
The specific embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
The inventor has carried out deep creative research and test to the present invention, and many successful embodiment are arranged, and enumerates four specific embodiments below.
Embodiment one
The first step is got the 100 treated soybean germs of gram (180 ℃ heat treated 15 minutes), adds 500 milliliters water, and slight boiling condition is extraction 30 minutes (stirrings) down, coextraction always three times, and after the filtered through gauze, merging filtrate gets about 1200 milliliters.
Second step through smart filter or centrifugal after, obtain clarification filtration liquid or supernatant.
The 3rd step was made hyperfiltration treatment to the supernatant of the second step gained, and the molecule interception of milipore filter is 10,000, and film type is a CAM.The ultrafiltration mode adopts intermittent operation, divides three steps: 1200 milliliters → 300 milliliters; Add water to 600 milliliters, 600 milliliters → 300 milliliters (secondary).Get about 1500 milliliters of ultrafiltrate altogether.
The 4th step ultrafiltrate is concentrated into about 50 milliliters through vacuum, moves to beaker again, evaporation and concentration under normal temperature, and the paste 10.3 that must be rich in isoflavones restrains (solid content is about 50%, and isoflavone content is about 15%).Color and luster is a pitchy, is transparent faint yellow to yellowish-brown after the dilution, and concentrate is little hardship, little puckery, however the pleasant impression sweetness.
Embodiment two
The first step is got 100 grams through heat treated soybean germ (180 ℃ heat treated 30 minutes), adds 500 milliliters water, 80 ℃ of extractions 3 hours (stirrings) down, and coextraction always three times, after the filtered through gauze, merging filtrate gets about 1200 milliliters.
Second step added a certain amount of fining agent (basic aluminium chloride), left standstill centrifugal after 24 hours (4000 rev/mins) under 4 ℃, collected centrifugate.Precipitation is used a spot of cold water washing, and is centrifugal once more, merges centrifugate.
The 3rd step centrifugate enters macroporous absorbent resin post (macroporous absorbent resin is NKB-12, and column volume is 200 milliliters) adsorbs, and flow velocity is (3～5) BV/ hour; Before the alcohol solvent wash-out, earlier with 3～4 BV of deionized water rinsing; Eluant, eluent employing percent by volume is 70% ethanolic solution, collects the eluting peak component.
The 4th step gained ethanol eluate is concentrated into certain volume through vacuum, and freeze drying again obtains the Powdered isoflavones of 5.2 grams, and wherein the purity of isoflavones is about 38%.This product color is a yellowish-brown, and it is little puckery to distinguish the flavor of, the pleasant impression sweetness.
Embodiment three
The first step is got the 100 treated soybean germs of gram (120 ℃ heat treated 60 minutes), adds 500 milliliters water, and slight boiling condition is extraction 60 minutes (stirrings) down, coextraction always three times, and after the filtered through gauze, merging filtrate gets about 1000 milliliters.
Second step added a certain amount of fining agent (basic aluminium chloride), and room temperature leaves standstill centrifugal after 6 hours (4000 rev/mins), collected centrifugate.Precipitation is used a spot of cold water washing, and is centrifugal once more, merges centrifugate.
The 3rd step centrifugate enters macropore absorption resin column (macropore absorption resin is X-5, and column volume is 200 milliliters) and carries out absorption, and flow velocity is (3～5) BV/ hour; Before the alcohol solvent wash-out, earlier with 3～4 BV of deionized water rinsing; Eluant, eluent employing percent by volume is 70% ethanolic solution, collects the eluting peak component.
The 4th step gained ethanol eluate is concentrated into certain volume through vacuum, and freeze drying again obtains the Powdered isoflavones of 5.8 grams, and wherein the purity of isoflavones is about 35%.This product color is khaki, bitterness, and pleasant impression is slightly sweet.
Embodiment four
The first step is got the 100 treated soybean germs of gram (180 ℃ heat treated 30 minutes), adds 500 milliliters water, and slight boiling condition is extraction 60 minutes (stirrings) down, coextraction always three times, and after the filtered through gauze, merging filtrate gets about 1200 milliliters.
Second step further through after the smart filter, was collected filtrate.
The 3rd step centrifugate enters macropore absorption resin column (macropore absorption resin is NKB-12, and column volume is 200 milliliters) and carries out absorption, and flow velocity is (3～5) BV/ hour; Before the alcohol solvent wash-out, earlier with the individual BV of deionized water rinsing (3～4); Adopting percent by volume in succession is that 40% and 70% ethanolic solution carries out wash-out, collects each eluting peak component respectively.
The 4th goes on foot the different ethanol eluates of gained, concentrates through vacuum and removes alcohol, and freeze drying again obtains 4.2 grams and the Powdered isoflavones of 1.4 grams respectively, and wherein the purity of isoflavones is about 42% and 33% respectively.The isoflavones sample that adopts 40% ethanol elution to obtain is yellowish-brown, and the pleasant impression sweetness is water-soluble good.The sample that 70% ethanol elution obtains also is yellowish-brown, and flavor is bitter, puckery.
Claims (5)
1. the production method of a sweet flavor isoflavones base-material is characterized in that it comprises the steps and process conditions:
The first step will be in dry soybean germ raw material 120～180 ℃ of following heat treated 15～90 minutes;
Second step is in soybean germ, according to the kilogram of raw material with total extractant: rising solid-to-liquid ratio 1: 8～15 adds water, in the extraction 0.5～3 hour down of 80 ℃～little fluidized state, filtration;
The 3rd step filtrate is left standstill after 6～24 hours under 4～25 ℃ centrifugal through clarification or filtration treatment;
Supernatant after the 4th step is centrifugal adopts hyperfiltration treatment, the molecule interception 10,000 of milipore filter, and the ultrafiltrate vacuum concentrates and gets final product.
2. the production method of a kind of sweet flavor isoflavones base-material according to claim 1 is characterized in that the heating condition of the described first step is 160～180 ℃ of following heat treated 20～45 minutes.
3. the production method of a kind of sweet flavor isoflavones base-material according to claim 1 is characterized in that, the extraction conditions in described second step is 90～95 ℃ and extracted 1～2 hour down that extractant is a water, filtered through gauze, merging filtrate behind the triplicate.
4. the production method of a kind of sweet flavor isoflavones base-material according to claim 1, it is characterized in that, the supernatant in described the 4th step enters the macroporous absorbent resin post and adsorbs, flow velocity is 3～5BV/ hour, adopt 3～4 BV of deionized water rinsing then, then carry out wash-out, eluant, eluent employing percent by volume is 40～70% ethanolic solution, and gained isoflavones eluent vacuum concentrates goes alcohol to get final product.
5. according to the production method of claim 1 or 4 described a kind of sweet flavor isoflavones base-materials, it is characterized in that, the isoflavones base-material that described the 4th step obtains is isoflavones liquid-type base-material or paste liquid base material, and further spray-drying makes powdered isoflavones base-material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031398952A CN1237896C (en) | 2003-07-18 | 2003-07-18 | Method for producing base material of soybean isoflavone with sugariness taste |
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| CNB031398952A CN1237896C (en) | 2003-07-18 | 2003-07-18 | Method for producing base material of soybean isoflavone with sugariness taste |
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| CN1480063A CN1480063A (en) | 2004-03-10 |
| CN1237896C true CN1237896C (en) | 2006-01-25 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105771313B (en) * | 2014-08-10 | 2017-11-24 | 嵊州北航投星空众创科技有限公司 | A kind of azalea extracting flavonoids system |
| CN110151817A (en) * | 2019-06-21 | 2019-08-23 | 三原利华生物技术有限公司 | The preparation method of water-soluble soybean isoflavone |
| CN113861152A (en) * | 2021-11-04 | 2021-12-31 | 山东东宇生态科技有限公司 | Preparation method of soybean isoflavone |
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