A kind of Maca extract removes sugared technique
Technical field
The present invention relates to a kind of except the method for sugar, more particularly to a kind of technique of Maca extract crystallization purifying oligosaccharides,
Belong to a kind of Maca extract concentration technique.
Background technology
Maca(Maca), it is Cruciferae(Cruciferae)Separate row Vegetable spp (Lepidium) is annual or biennial plant
Maca(L.meyenii Walp.)Root tuber, research shows, abundant vitamin, mineral matter, amino acid and meals are contained in maca
Fiber is eaten, and containing functional components such as abundant macamide, maca ene, glucosinolate, polysaccharide, sterols, has enhancing immune
Power, dispelling fatigue, improve sperm motility, treatment rheumatism, regulation endocrine, raising memory, treatment climacteric metancholia, anti-bone
The functions such as matter is loose, anticancer.
Monose is usually polyhydroxy aldehyde or polyhydroxyketone containing 3-6 carbon atom, and disaccharide is that the monose of two molecules passes through
What glycosidic bond was formed, polysaccharide is by multiple monosaccharide molecules are condensed, dehydration forms, and is the complicated and huge carbohydrate of molecule mechanism
Material, oligosaccharide are generally the sugar that 2~10 monose are connected to form with glycosidic bond, and monosaccharide and disaccharide or oligosaccharide are general all
Referred to as oligosaccharides.Monose and disaccharide can provide heat energy to human body, and form tissue and protect the important substance of liver function, but
Excess free enthalpy can cause the diseases such as obesity, artery sclerosis, hypertension, diabetes and carious tooth, and oligosaccharide and polysaccharide typically have
Very strong antiviral activity, antitumor activity, anti-inflammatory activity, antioxidation activity and the immune three high drop effect of regulation.
Also there are some crystal sugar techniques to can be used for extract except sugar now, as authorized Publication No. CN103060482A
In Chinese patent, a kind of technique of production of corn starch crystal diabetin is disclosed, fructose is made in the technology utilization glucose, and leads to
Cross chromatographic isolation and obtain the higher aqueous solution of purity, then when row vacuum evaporating crystalization.And for example Publication No. CN102992957A
In Chinese patent, a kind of dilution crystallization method of antierythrite is disclosed, the handy dissolved agent of this method is crystallized, can obtained
The higher sugar alcohol product of quality.For another example Authorization Notice No. is in CN10253453B Chinese patent, discloses a kind of raising xylose
The method of crystallization yield, the mode of the handy gradient cooling of this method, to improve crystallization yield.
Maca is external advantitious plant, and new resource food was approved as by the Ministry of Public Health in 2011, up to the present domestic
Study less, do not there is special polysaccharide purification method.The existing carbohydrate crystallization purifications of above and other, there is or work
Skill is more complicated, cost is higher, or needs to add the reason such as dissolved agent, security difference that can not be eaten, and is not fully applied to
Maca removes sugared technique.
In summary, there is presently no a kind of simple to operate, cost is low, and device simple, energy consumption is low, and purity is high, security
It is good, it can guarantee that the loss-free Maca extract of functional component removes sugared purification process.
The content of the invention
It is an object of the invention to overcome above shortcomings in the prior art, and provide a kind of simple to operate, cost
Low, device simple, energy consumption is low, and purity is high, and security is good, can guarantee that the loss-free Maca extract of functional component removes sugared technique.
Technical scheme is used by the present invention solves the above problems:The Maca extract is removed the characteristics of sugared technique and is:
The technique comprises the following steps:
(1) maca extract is placed in vacuum concentrator, at 35~50 DEG C of temperature, 5~12Kpa pressure, concentration
Extractant is reclaimed, obtains concentrated extract;
(2) concentrated extract that step (1) obtains is dissolved in edible ethanol, the weight of edible ethanol used is soaked for concentration
15~25 times of cream weight, stir, and in faint yellow clear solution, the solution are placed in vacuum rotary evaporator, 35
DEG C temperature, under 12Kpa pressure, be concentrated into that volume is concentrated extract 3~10 times, obtain Maca extract ethanol solution;
(3) the Maca extract ethanol solution that step (2) obtains is placed in interlayer crystallizing tank, stand at low temperature 24~48 is small
When;
(4) it is even with 60 turns/min speed at a temperature of the Maca extract ethanol solution after standing being placed in into -5~10 DEG C
Speed stirring 30min, while stirring, ultrasonic wave is applied to Maca extract ethanol solution;
(5) the Maca extract ethanol solution in step (4) is stood 6~24 hours, filtering, obtains crystal sugar and ethanol
Solution is 1.;
(6) crystal sugar is dissolved in edible ethanol, the weight of edible ethanol used is 7-13 times of crystallization sugar weight, weight
Multiple step (3)~(5) twice, obtain recrystallization sugar, ethanol solution 2. with ethanol solution 3.;
(7) mixed ethanol solution 1., ethanol solution 2. with ethanol solution 3., be placed in concentrating in vacuum concentrator, obtain
Except the Maca extract medicinal extract of sugar.
So that the present invention can effectively ensure maca ene, the maca contained in Maca extract while except sugar
The functional components such as acid amides and sulphur glycoside do not lose, whole technical process it is simple to operate, cost is low, and device simple, energy consumption is low,
Purity is high, and security is good.
Preferably, the maca extract in step (1) of the present invention is maca ethanol extract or maca ethanol water
Mixed extract.
Preferably, in step (2) of the present invention, be concentrated into that volume is concentrated extract 3~5 times.
Preferably, in step (3) of the present invention, temperature that Maca extract ethanol solution is stood in interlayer crystallizing tank
Spend for 5~15 DEG C.
Preferably, in step (4) of the present invention, supersonic frequency is between 20~50kHz.
The present invention compared with prior art, has advantages below and effect:(1)Whole technique is molten only with edible ethanol
Agent, it is safe.(2)Sugared container is removed as crystallization using single interlayer crystallizing tank, cooled beneficial to solution, equipment is simple, cost
Low, operation is easy.(3)Carbohydrate crystallization nucleation in Maca extract is accelerated using ultrasonic wave, saves the time.(4)While nucleation,
Using agitating mode, avoid nucleus from being bonded on crystallization tank skin, influence crystal and separated with solution.(5)Purity is high, and active principle is lossless
Lose, after recrystallizing three times, the purity of the maca crystal sugar of acquisition is up to more than 99%, and effective component in Maka loss is less than
Less than 0.5%;Inventor research shows, in maca root tuber containing mass percent be 3~8% polysaccharide and 17~24% oligosaccharides,
The present invention be in order to which oligosaccharides purifies and separates in Maca extract, liquid chromatographic detection result and molecular weight analysis result are shown,
Maca crystal sugar is mainly glucosyl group monosaccharide and disaccharide and trisaccharide, wherein based on maltose, can be slightly soluble in ethanol.Maca
In extract in addition to the oligosaccharides containing 1~3 monose, also containing functional components such as maca ene, macamide and sulphur glycosides,
The present invention is and effective while except sugar primarily to remove the glucosyl group monosaccharide and disaccharide and trisaccharide in Maca extract
It ensure that the functional components such as maca alkenes, macamide class, maca sulphur glycoside, maca sterols, maca polysaccharide class do not lose.
Brief description of the drawings
Fig. 1 is monose derivatization standard sample of embodiment of the present invention HPLC figures, wherein, 12~13min peaks are glucose.
Fig. 2 is Maca extract crystal sugar of embodiment of the present invention simple monosaccharide composition HPLC figures.
Embodiment
Below in conjunction with the accompanying drawings and the present invention is described in further detail by embodiment, and following examples are to this hair
Bright explanation and the invention is not limited in following examples.
Embodiment 1.
Maca extract in the present embodiment comprises the following steps except sugared technique.
(1) maca extract at 35~50 DEG C of temperature, 5~12Kpa pressure, is concentrated back in vacuum concentrator
Receive extractant.Maca extract in the present invention can be the ethanol extract or water alcohol mixed extract of maca, the water of maca
Alcohol mixed extract refers to the extract solution obtained with ethanol water extraction maca.By maca extract in low temperature, the ring of low pressure
Under border, extractant is reclaimed, concentrated extract is obtained, contains maca ene, macamide and sulphur glycoside functional component in the concentrated extract,
And substantial amounts of sugared part.
(2) concentrated extract that step (1) obtains is dissolved in edible ethanol, the weight of edible ethanol used is 15~25
Times concentrated extract weight, stir, in faint yellow clear solution, in vacuum rotary evaporator, 35 DEG C of temperature,
Under 12Kpa pressure, by 3~10 times of volume concentration to concentrated extract volume.Concentrated extract is dissolved in pure edible ethanol,
The dissolving of stirring auxiliary, ultrasonic wave added dissolving can be used if necessary, concentrated extract is completely dissolved in ethanol, Maca extract
Ethanol solution now contains macamide, maca ene, sulphur glycoside compound and carbohydrate, is carbohydrate typically in light yellow in solution
Unsaturated solution.The carbohydrate unsaturated solution of Maca extract is concentrated into body in 35 DEG C of temperature, 12Kpa vacuum under pressure
Product is 3~10 times of concentrated extract, forms the supersaturated solution of carbohydrate.
(3) the Maca extract ethanol solution for obtaining step (2), is placed in interlayer crystallizing tank, stand at low temperature 24~48
Hour;Under normal circumstances, Maca extract ethanol solution is poured into interlayer crystallizing tank, interlayer leads to coolant, coolant temperature
Between 5~15 DEG C, 24~48 hours are stood, supersaturated sugar juice is down to required temperature, whole solution system, temperature completely
It is stable.
(4) the maca ethanol solution stood is at the uniform velocity stirred at a temperature of -5~10 DEG C with 60 turns/min speed
30min, while stirring, apply 20~50kHz frequency ultrasonic waves to solution and promote the nucleus of sugar to produce, optimal supersonic frequency is
25~35kHz, can make that nucleus quickly forms and basic growing the grain terminates within 5min, solution be applied low while ultrasonic wave
Speed stirring, is to prevent from being formed a large amount of nucleus and long great achievement crystal on chamber wall, cause next step solution to be separated with crystal tired
It is difficult.Using high-speed stirred supersaturated maca ethanol sugar juice nucleus can also be promoted to be formed, but mixing speed will be in 800 turns/min
More than, this is easily realized in laboratory conditions, industrialized large scale equipment, so high rotating speed, is caused between blade and solution
High shear force, be easy to promote nucleus to be formed, but also easily cause the temperature of solution to rise, hinder the formation of nucleus on the contrary,
Invention promotes nucleus to be formed using ultrasound, and stirring at low speed prevents wall from crystallizing, and can quickly form nucleus, and and can is prevented in temperature
Rise.
(5) solution left standstill for obtaining step (4) 6~24 hours, filtering, isolated crystal sugar and ethanol solution are 1.;
Under normal circumstances, the solution after the nucleus of step (4) acquisition is formed stands growing the grain 6~24 hours, made at a temperature of 5~15 DEG C
Crystal is formed completely, the valve for crystallizing pot bottom is opened, filtering, the maca ethanol extraction of isolated crystal sugar and desugar
Liquid, i.e. crystal sugar and ethanol solution are 1..
(6) crystal sugar in step (5) is redissolved in the edible ethanol of 10 times of crystallization sugar weights, repeat step (3)
~(5) twice, obtain recrystallization sugar, ethanol solution 2. with ethanol solution 3..The nucleus of partially crystallizable sugar may be having for maca
Ingredient granules are imitated, part active ingredient can be also wrapped in the inside in sugared crystallization process, repeat to dissolve recrystallization process twice, can
To obtain purity up to 99% crystal sugar.
(7) ethanol solution that blend step (5) and (6) obtain 1., ethanol solution 2. with ethanol solution 3., in vacuum concentration
Concentrate, obtained except the Maca extract medicinal extract of sugar in device.Generally look at down, by the maca ethanol solution that Crystallization Separation three times arrives in
It is concentrated in vacuo in container, 35 DEG C of temperature, under 12Kpa pressure, reclaims ethanol completely, obtain except the Maca extract medicinal extract of sugar.
Show that maca crystal sugar is mainly grape by Fig. 1 and Fig. 2 liquid chromatographic detection result and molecular weight analysis result
Glycosyl monosaccharide and disaccharide and trisaccharide, wherein based on maltose, ethanol can be slightly soluble in.
Embodiment 2.
Maca extract in the present embodiment comprises the following steps except sugared technique.
(1) take 100Kg macas dry sliced, be crushed to 200 mesh, pour into ultrasonic extraction kettle, add 500Kg volume hundred
Divide than the edible ethanol for 80%, ultrasonic extraction 3 times, merge extract solution, obtain 1600Kg maca ethanol water mixed extracts altogether.
(2) maca ethanol water mixed extract is poured into continous way Rotary Evaporators, in 35 DEG C of temperature, 10Kpa pressure
Vacuum under, concentration and recovery ethanol, at 40 DEG C of temperature, the vacuum of 8Kpa pressure, concentration and recovery water, obtain the contracting of 22Kg concentrates
Medicinal extract.
(3) concentrated extract is dissolved in 440Kg edible ethanol, stirred, in faint yellow clear solution, then will dissolving
Good edible ethanol solution is placed in continuous vacuum Rotary Evaporators, 35 DEG C of temperature, and under 12Kpa pressure, volume concentration is extremely
120 liters.
(4) the 120L maca ethanol solutions in step (3) are placed in interlayer crystallizing tank, the logical 10 DEG C of coolings of crystallizing tank interlayer
Liquid, stand at low temperature 24 hours.
(5) crystallizing tank coolant temperature is adjusted to -5 DEG C of temperature, after stable, maca is at the uniform velocity stirred with 60 turns/min speed
Ethanol solution 30min, while stirring, apply 35KHz ultrasonic wave to solution, fine crystalline body is formed in solution.
(6) by the solution left standstill that is obtained after ultrasound 12 hours, make that crystal sugar crystallization is complete, and filtering, separation obtains crystal sugar
20Kg and ethanol solution 1. 100L.
(7) by step(6)The crystal sugar of middle acquisition is redissolved in 200L edible ethanol, repeat step (4)~(6) two
It is secondary, obtain recrystallize sugared 19.9Kg, ethanol solution 2. with ethanol solution 3., volume of the ethanol solution 2. with ethanol solution 3. adds up to
400L。
(8) ethanol solution that blend step (6) and (7) obtain 1., ethanol solution 2. 3. add up to 500L with ethanol solution, in
In continous way Rotary Evaporators, 35 DEG C of temperature, under 12Kpa pressure, recovery ethanol is concentrated in vacuo, obtains the maca extraction except sugar
Thing medicinal extract 2Kg, in medicinal extract macamide and maca ene content more not except it is sugared when improve 10 times.
Show that maca crystal sugar is mainly grape by Fig. 1 and Fig. 2 liquid chromatographic detection result and molecular weight analysis result
Glycosyl monosaccharide and disaccharide and trisaccharide, wherein based on maltose, ethanol can be slightly soluble in.
Embodiment 3.
Maca extract in the present embodiment comprises the following steps except sugared technique.
(1) 500Kg maca xeraphiums are taken, are poured into ultrasonic extraction kettle, add 3000Kg edible ethanol, ultrasonic extraction 3
It is secondary, merge extract solution, obtain 9500Kg maca ethanol extracts altogether.
(2) maca ethanol extract is poured into continous way Rotary Evaporators, in 35 DEG C of temperature, the vacuum of 10Kpa pressure
Under, concentration and recovery ethanol, volume concentration is to 1000 liters.
(3) 1000L maca ethanol solutions are placed in interlayer crystallizing tank, crystallizing tank interlayer leads to 5 DEG C of coolants, stand at low temperature
48 hours.
(4) crystallizing tank coolant temperature is adjusted to 0 DEG C of temperature, after stable, maca is at the uniform velocity stirred with 60 turns/min speed
Ethanol solution 30min, while stirring, apply 25KHz ultrasonic wave to solution, fine crystalline body is formed in solution, and crystallize
The basic nodeless mesh of tank skin.
(5) by the solution left standstill that is obtained after ultrasound 24 hours, make that crystal sugar crystallization is complete, and filtering, separation obtains crystal sugar
95Kg and ethanol solution 900L.
(6) crystal sugar obtained in step (5) is redissolved in 1000L edible ethanol, repeat step (3)~(5)
Twice, obtain and recrystallize sugared 94Kg and ethanol solution 2000L.
(7) the ethanol solution 2900L that blend step (5) and (6) obtain, in continous way Rotary Evaporators, 35 DEG C of temperature,
Under 12Kpa pressure, be concentrated in vacuo recovery ethanol, obtain except the Maca extract medicinal extract 7.5Kg of sugar, in medicinal extract macamide and
Maca ene content improves 12 times when not removing sugared.
Show that maca crystal sugar is mainly grape by Fig. 1 and Fig. 2 liquid chromatographic detection result and molecular weight analysis result
Glycosyl monosaccharide and disaccharide and trisaccharide, wherein based on maltose, ethanol can be slightly soluble in.
Embodiment 4.
Maca extract in the present embodiment comprises the following steps except sugared technique.
(1) maca extract is placed in vacuum concentrator, at 35~50 DEG C of temperature, 5~12Kpa pressure, concentration
Extractant is reclaimed, obtains concentrated extract.Maca extract in step (1) can be maca ethanol extract or maca ethanol water
Mixed extract.
(2) concentrated extract that step (1) obtains is dissolved in edible ethanol, the weight of edible ethanol used is soaked for concentration
15~25 times of cream weight, stir, and in faint yellow clear solution, the solution are placed in vacuum rotary evaporator, 35
DEG C temperature, under 12Kpa pressure, be concentrated into that volume is concentrated extract 3~10 times, obtain Maca extract ethanol solution.This
Invention can be concentrated into 3~5 times that volume is concentrated extract.
(3) the Maca extract ethanol solution that step (2) obtains is placed in interlayer crystallizing tank, stand at low temperature 24~48 is small
When.The temperature that Maca extract ethanol solution is stood in interlayer crystallizing tank can be 5~15 DEG C.
(4) it is even with 60 turns/min speed at a temperature of the Maca extract ethanol solution after standing being placed in into -5~10 DEG C
Speed stirring 30min, while stirring, ultrasonic wave is applied to Maca extract ethanol solution.Supersonic frequency can be in 20~50kHz
Between.
(5) the Maca extract ethanol solution in step (4) is stood 6~24 hours, filtering, obtains crystal sugar and ethanol
Solution is 1..
(6) crystal sugar is dissolved in edible ethanol, obtains crystal sugar ethanol solution, the weight of edible ethanol used is knot
7-13 times of pied-de-cuite weight.
(7) the crystal sugar ethanol solution that step (6) obtains is placed in interlayer crystallizing tank, stand at low temperature 24~48 hours.
The temperature that crystal sugar ethanol solution is stood in interlayer crystallizing tank can be 5~15 DEG C.
(8) at a temperature of the crystal sugar ethanol solution after standing being placed in into -5~10 DEG C, at the uniform velocity stirred with 60 turns/min speed
Mix 30min, while stirring, ultrasonic wave is applied to crystal sugar ethanol solution.Supersonic frequency can be between 20~50kHz.
1. and ethanol (9) the crystal sugar ethanol solution in step (8) is stood 6~24 hours, filtering, obtains recrystallization sugar
Solution is 2..
(10) 1. recrystallization sugar is dissolved in edible ethanol, obtains recrystallizing sugared ethanol solution, edible ethanol used
Weight, which is attached most importance to, crystallizes 7-13 times of sugar weight.
(11) the recrystallization sugar ethanol solution that step (10) obtains is placed in interlayer crystallizing tank, stand at low temperature 24~48 is small
When.It can be 5~15 DEG C to recrystallize the temperature that sugared ethanol solution is stood in interlayer crystallizing tank.
(12) at a temperature of the recrystallization sugar ethanol solution after standing being placed in into -5~10 DEG C, with 60 turns/min speed at the uniform velocity
30min is stirred, while stirring, counterweight crystal sugar ethanol solution applies ultrasonic wave.Supersonic frequency can 20~50kHz it
Between.
(13) by step (12) recrystallization sugar ethanol solution stand 6~24 hours, filtering, obtain recrystallization sugar 2. and
Ethanol solution is 3..
(14) mixed ethanol solution 1., ethanol solution 2. with ethanol solution 3., be placed in concentrating in vacuum concentrator, obtain
Except the Maca extract medicinal extract of sugar.
Show that maca crystal sugar is mainly grape by Fig. 1 and Fig. 2 liquid chromatographic detection result and molecular weight analysis result
Glycosyl monosaccharide and disaccharide and trisaccharide, wherein based on maltose, ethanol can be slightly soluble in.
Although the present invention is disclosed as above with embodiment, it is not limited to protection scope of the present invention, any ripe
The technical staff of this technology is known, in the change and retouching made without departing from the spirit and scope of the invention, this all should be belonged to
The protection domain of invention.