CN1164600C - Process for preparing bifidobacterium factor oligose from gestumor tuber - Google Patents
Process for preparing bifidobacterium factor oligose from gestumor tuber Download PDFInfo
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- CN1164600C CN1164600C CNB011096926A CN01109692A CN1164600C CN 1164600 C CN1164600 C CN 1164600C CN B011096926 A CNB011096926 A CN B011096926A CN 01109692 A CN01109692 A CN 01109692A CN 1164600 C CN1164600 C CN 1164600C
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Abstract
The present invention relates to a method for preparing bifidobacterium factor oligose with stachyose as a main component by gestumor tubers which belong to special betony in the dry regions and semiarid regions of China. The method comprises the technological processes of pre-treating the gestumor tubers, thermal extracting in deionized water, removing dregs and impurities, decoloring, filtering, refining, concentrating and spray drying, etc. The present invention has the advantages of stable preparation quality, high purity, good health-care function of bifidobacterium factor oligose, low cost, high yield and full utilization of resources.
Description
Technical field
The present invention relates to a kind of method for preparing the bifidus factor oligose in the middle of Chinese medicine Herba Lycopi's the piece root, belong to the field of Chinese medicines.
Background technology
" gestumor " is ground bamboo shoot or Herba Lycopi's piece or root, bar root shape cry herbvore silkworm, China's western arid area custom is referred to as gestumor.This type of plant is starch-containing hardly, and its main component is that moisture content is about 78%, and crude protein is about 2.6%, crude fat 0.1%, soluble solid is about 16%, other 3.3%, wherein contain the oligose of 12-15% of having an appointment based on stachyose (stackyose).In the past, among the peoplely more are used for making salted vegetables or make the animal feed.If oligose extraction separation that will be wherein, making functional foodstuff or medicine has very important meaning and good economic benefits, social benefit.The bifidus factor oligose generally is meant the general name that contains raffinose (trisaccharide), stachyose (tetrose) and sugarcane chaff, glucose, fructose etc.It has tangible proliferation function to the intravital probiotics bifidus bacillus of people.This class sugar extensively is present in the plant, and extracting method is different because of different raw materials.When being raw material with the soybean, general with the molten acid cure method of alkali or use through quintessence and follow the example of, this preparation method technical process complexity, refining difficulty is big: and for example the oligose of producing with corn must transform with allomerase, and these enzymes also need import at present, technological process is also comparatively complicated, implements certain difficulty in industrial under-developed area.
Summary of the invention
Therefore, the present invention seeks to provide a kind of method for preparing the bifidus factor oligose in the middle of Chinese medicine Herba Lycopi's the piece root in order to develop western resource.
Technical scheme of the present invention comprise raw material pre-treatment, extract, remove slag, removal of impurities, decolouring, filtration, refining, concentrate, step such as powdered.
At first, clean up after the fresh feed purchase, thoroughly remove sandy soil and impurity.In order to prevent that raw material from brown stain taking place in drying process,, held time 5-10 minute with the big gun of 0.1-0.2Mpa and the steam enzyme that goes out.In this course, not only can destroy the activity of various enzymes, and can make protein denaturation, help the separation of sugar part.The raw material behind the enzyme of then will going out is dried or is dried and stores for future use.
With the material coarse cutting of oven dry, drop into extractor, add 6-10 doubly to the deionized water of raw material weight.Raw material granularity after the coarse crushing is the 1-5 millimeter, and the deionization electrical conductivity of water is 10-100us/cm, is heated to 60-100 ℃, stirs and extracts 20-120 minute.Filter residue after the extraction drains juice through squeezing machine to be mixed with extracting solution.In mixed solution, add the acidic white earth account for filtrate weight 1-5% then, stir, left standstill 1-8 hour, allow wherein protein and colloidalmaterial coagulation sedimentation.Then with flame filter press or ultra-filtration equipment carry out essence filter clear solution.
Though the transparent clarification of the liquid glucose after the filtration wherein still contains coloring materials such as a spot of protein, colloidalmaterial, metal ion, so need to decolour with gac.Use the granular carbon of particle diameter as 0.5-1.0mm, consumption is liquid glucose amount 1-3%, under 50-80 ℃, insulated and stirred 10-20 minute, leaves standstill 10-30 minute.
The filtration step that the present invention adopts can also be: adopt flame filter press to filter, with 150-200 purpose filter cloth, form filter cake on the filter cloth for making, adding accounts for liquid weight 0.5-5% diatomite in destainer, circulate and filter repeatedly, till clear.
Then, filter with flame filter press.Use 150-200 order filter cloth.In the decolouring liquid glucose, add the diatomite of 0.5-5% before filtering, filter while stirring, until the liquid glucose that obtains clear.
Treating process is that employing macroporous resin and anion and cation exchange resin are the separation and purification material.Specifically be adopt macroporous ion exchange resin and anion and cation exchange resin totally 4 ion exchange columns series connection make with extra care.In first ion exchange column, pack into and account for 800 type macroporous resins of its volume 75%, second exchange column is packed into and is accounted for 732 type Zeo-karbs of its volume 75%, the 3rd exchange column is packed into and is accounted for 717 type anionite-exchange resin of its volume 75%, 717 type anionite-exchange resin and 732 type Zeo-karbs that the 4th exchange column is packed into and accounted for its volume 75%, and the ratio of anionite-exchange resin and Zeo-karb is 6:4, and the liquid glucose flow rate control is in 1-2 times of exchange resin volume.
Sugar concentration after ion exchange resin is refining is lower, and should be concentrated into soluble solid content is 30---45%, capable again spraying drying.Concentrate to adopt the film type vacuum concentration equipment, vacuum degree control is at 600---650mmHg, about about 60 ℃ of temperature.
At last, the liquid glucose after concentrating is carried out spraying drying, during spraying, the inlet temperature of material is 130---160 ℃, and the temperature out of product is 60---80 ℃.
The powder-product that present technique is produced detects through high performance liquid chromatography, and the above oligosaccharide contg of trisaccharide reaches 60---90%, because of the kind of raw material different and different with the place of production.
The advantage of the inventive method is:
1, pass through the refining of macroporous resin regulating YIN and YANG ion exchange resin, wherein the packing height of resin column is 75%, makes the purity of product improve greatly;
2, because the inventive method is not used ethanol, reduced cost to a great extent, and water refluxing extraction method controls easily, cut the waste;
3, the present invention is a raw material with the autochthonal plant Herba Lycopi's of western arid area piece root, and not only cost is low, and makes full use of local resources, has good economic benefits and social benefit.
4, the oligose product of Ti Quing based on stachyose, has purposes widely, shows:
(1) as the diet sweeting agent of specific crowd
Because it is difficult to be absorbed by human consumption,, can not cause the rising of edible back blood glucose value so the Energy value that he can provide is very low or energy is not provided yet.Like this, just be specially adapted to those obese persons that have a sweet tooth, diabetics and worry that sugar causes that too much the people of adverse consequences are edible as sweeting agent.Obtained widespread use in this respect.
(2) as the activation factor of bifidus bacillus
Bifidus bacillus is the normal probiotics of settling down in the human intestinal, promotes aspects such as infant growth, delaying human body caducity to play an important role to keeping HUMAN HEALTH.A couple of days behind the baby due, the quantity of bifidus bacillus just begins to preponderate in the enteron aisle, can reach more than 90% of intestinal microflora.After infancy, with advancing age.This bacterium quantity can reduce gradually.When the people arrived old age, bifidus bacillus reached extremely low quantity entirely.Simultaneously, some patient also often causes normal microflora equilibrated destruction in the body because of the microbiotic of life-time service broad-spectrum high efficacy, produces so-called normal microflora deficiency disorder.On purpose keeping probiotics, the particularly bifidus bacterium quantity in enteron aisle is one of important assurance of keeping HUMAN HEALTH, and this point has caused the great attention of microecology man.People discover that the activation of bifidobacterium growth breeding needs a kind of so-called bifidus factor, and it is exactly in fact some oligose.The surface of bifidus bacillus may have the bifidus factor acceptor, can be specifically with these oligosaccharide acts and absorb it, and activate certain biological process.Such as, it is found that, contain the oligose of a kind of N-acetyl-D-glucosamine in the human milk, by bifidus bacillus synthetic cell wall essential.Many oligose activate bifidobacterium growths and breed that the cutter reason is also not really clear really, but studies show that their promotes growth effect is sure fully really.
(3) anti-dental caries effect
Many table sugar can be utilized by oral microorganism or decompose, and cause the tooth pathology.Carious tooth is exactly that streptococcus mutans (streptococcus mutans) erosion that exists in the oral cavity causes.Oligose is not their suitable effect substrates generally not for these Institute of Micro-biology decompose, and can not cause that therefore the tooth dental caries become.Therefore, the active oligose with pure sweet taste is specially adapted to candy, especially the manufacturing of children candies.
(4) has the function of food fibre
Because active oligose is by human consumption, also can be regarded as water-soluble dietary fibre, the function same with food fibre arranged, can reduce the generation of toxic substance, prevention colorectal carcinoma in cholesterol in the serum, the absorption intestines etc.It has different again with high molecular food fibre simultaneously.Because it has sweet taste more, molecular weight is lower, so be widely used in beverage, food.
Experimental example carries out stratographic analysis according to following method to products obtained therefrom:
1, instrument: U.S. waters high performance liquid chromatograph, 510 pumps, R401 differential refraction detector, WDL-95 chromatographic working station.
2, the preparation of sample: concentration of standard solution is 0.2%, and sample solution concentration is 5%.
3, chromatographic condition:
Post: Spherisorb-HN2,300mm * 5mmi.d.
Detector sensitivity: 4 *
Moving phase: acetonitrile-water (70: 30) (moving phase is through 0.3 μ m filtering with microporous membrane, vacuum decoloration)
Flow velocity: 2.2ml/min
Sample size: 40 μ l
Temperature: 50 ℃
4, two kinds of sample A and B analytical results are as follows:
More than the sample title sucrose raffinose stachyose pentasaccharides
A 12.43 6.62 77.86 2.89
B 8.38 12.88 29.64 31.75
Description of drawings
Accompanying drawing 1 is the liquid-phase chromatographic analysis figure of sample A;
Accompanying drawing 2 is liquid-phase chromatographic analysis figure of sample B.
Embodiment
Embodiment 1
What (1) produce with the Northwest is raw material in " Chinese medicine Herba Lycopi's piece root ", take by weighing siccative 1kg, it is the 1-5mm size that coarse crushing becomes particle diameter, adds deionized water 10kg, together goes into to extract pot, be heated to 80 ℃, insulated and stirred 30 minutes, with the 80 eye mesh screens 5.5kg that filters to get filtrate, again filter residue is squeezed filtrate 2.1kg, altogether liquid glucose 7.6kg, record 6.5Be with hand-held saccharometer.In above-mentioned liquid glucose, add 0.1 kilogram of acidic white earth, left standstill after stirring 4 hours, be added with the diatomaceous suction filtration device of flocculating aids filter clear filtrate 7.0kg.
(2) add 75 gram granulated active carbons in above-mentioned liquid glucose, be heated to 70 ℃, insulated and stirred 10 minutes left standstill 30 minutes, added 100 gram diatomite then, stirred.
(3) load onto 200 purpose filter clothes with small-sized flame filter press, top decolouring liquid glucose is carried out circulating filtration, till the transparent clarification of liquid glucose.
(4) above-mentioned liquid glucose is heated to 50 ℃, adjusts pH value, it is kept between the 3.5-4.5, follow the ion exchange column of flowing through and anticipating and assemble in exchange resin 1-2 flow velocity doubly with per minute, effusive liquid glucose is as clear as crystal, at this moment, concentration is 6.2 kilograms of the liquid glucoses of 5.5 ° of Be.
(5) above-mentioned liquid glucose is carried out low-temperature evaporation with the film vacuum-evaporator and concentrate, vacuum tightness is 650mmHg, about 60 ℃ of temperature.Being concentrated into sugared concentration is about 1000 milliliters of 35 ° of Be.
(6) above liquid glucose is carried out spraying drying, the liquid glucose inlet temperature is 140 ℃, and the temperature out of product is 80 ℃, and the product of gained is about 250 grams of white powder.
(7) this white powder is through using high-performance liquid chromatogram determination, and the oligosaccharide contg more than the trisaccharide of warding off based on wood is 68.4%.
Embodiment 2:
The strip of producing with the North China " Chinese medicine Herba Lycopi's piece root " is a raw material.Clean through clear water, heat the enzyme that went out in 10 minutes with saturation steam and handle, again it is dried under the temperature about 60 ℃ to water content 5-8%, test (average 5 kilograms of bright raw materials can make the dried raw material of 1kg) with this dried raw material.
(1) takes by weighing the dried raw material of 1kg, be broken into the 1-5 millimeter-sized particles, place and extract pot, add the 10kg deionized water, be heated to 8 ℃, 60 minutes (this siccative is more solid) extracted in insulation, with the 80 eye mesh screens 61kg that filters to get filtrate, again filter residue is squeezed liquid glucose 1.8kg, altogether liquid glucose 7.9kg, pol is 7.0 ° of Be, in liquid glucose, add the 0.1kg acidic white earth then, stir, leave standstill 4 hours after, with oily filter device filter clarifying sugar liquid 7.5kg.
(2) (3) (4) step is identical with embodiment one, and the gained liquid glucose is 6.0kg after (4) treatment on ion exchange columns, and pol is 6.2 ° of Be.
(5) with (4) gained liquid glucose film vacuum-evaporator, be 600-650mmHg in vacuum tightness, temperature is that to be concentrated into pol under 55-60 ℃ be 38 ° of Be, about 1000ml.
(6) liquid glucose after (5) are concentrated carries out after the spraying drying to such an extent that product be a white powder, totally 280 grams.
(7) this product high-performance liquid chromatogram determination is 91.3% based on the oligosaccharide contg more than the trisaccharide of stachyose.
Claims (4)
1, a kind of method for preparing the bifidus factor oligose in the middle of Chinese medicine Herba Lycopi's the piece root, it is characterized in that comprising raw material pre-treatment, extract, remove slag, removal of impurities, decolouring, filtration, refining, concentrate, the powdered step; The removal step that removes slag is a method of taking coarse filtration and smart filter to combine: after removing thick slag with filter screen, in filtrate, add the acidic white earth that accounts for filtrate weight 1-5%, left standstill after stirring 1-8 hour, allow wherein protein and colloidalmaterial coagulation sedimentation, add flocculating aids then and carry out the essence filter through flame filter press, liquid glucose is passed through smoothly, and clear.
2, method according to claim 1, it is characterized in that said filtration step is to adopt flame filter press to filter, with 150-200 purpose filter cloth, form filter cake on the filter cloth for making, in destainer, add and account for liquid weight 0.5-5% diatomite, circulate and filter repeatedly, till clear.
3, method according to claim 1, it is characterized in that said making with extra care is to adopt macroporous ion exchange resin and the moon, positively charged ion changes the resin series connection and makes with extra care, in first ion exchange column, pack into and account for 800 type macroporous resins of its volume 75%, second exchange column is packed into and is accounted for 732 type Zeo-karbs of its volume 75%, the 3rd exchange column is packed into and is accounted for 717 type anionite-exchange resin of its volume 75%, 717 type anionite-exchange resin and 732 type Zeo-karbs that the 4th exchange column is packed into and accounted for its volume 75%, and the ratio of anionite-exchange resin and Zeo-karb is 6: 4, and the liquid glucose flow rate control is in 1-2 times of exchange resin volume.
4, method according to claim 1, it is characterized in that said enrichment step is to adopt the film vacuum-evaporator to concentrate, vacuum tightness 600-650mmHg, about 60 ℃ of temperature, syrup concentration after concentrating is 30-45 ° of Be, said powdered is to adopt spray-drying process to carry out drying, and the inlet temperature of material is 130-160 ℃, and the temperature out of material is 60-80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011096926A CN1164600C (en) | 2001-03-20 | 2001-03-20 | Process for preparing bifidobacterium factor oligose from gestumor tuber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011096926A CN1164600C (en) | 2001-03-20 | 2001-03-20 | Process for preparing bifidobacterium factor oligose from gestumor tuber |
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| CN1317492A CN1317492A (en) | 2001-10-17 |
| CN1164600C true CN1164600C (en) | 2004-09-01 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1260252C (en) | 2004-01-15 | 2006-06-21 | 华南理工大学 | Method for controlling molecular weight distribution of starch sugar |
| CN1273610C (en) | 2004-01-15 | 2006-09-06 | 华南理工大学 | Method for dispelling monosaccharide component from oligosaccharide |
| CN101633676B (en) * | 2009-06-04 | 2011-06-08 | 中国食品发酵工业研究院 | Method for preparing high-purity stachyose by using plant chromatographic separation technology |
| CN103265583B (en) * | 2013-03-05 | 2016-01-13 | 中国食品发酵工业研究院 | A kind of preparation method of stachyose crystal |
| CN104262418B (en) * | 2014-09-26 | 2017-04-19 | 何龙 | Production method of crystallized water threose |
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