CN104621436A - Maca extract sugar-removing technology - Google Patents
Maca extract sugar-removing technology Download PDFInfo
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- CN104621436A CN104621436A CN201410530392.2A CN201410530392A CN104621436A CN 104621436 A CN104621436 A CN 104621436A CN 201410530392 A CN201410530392 A CN 201410530392A CN 104621436 A CN104621436 A CN 104621436A
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- extract
- ethanolic solution
- maca extract
- maca
- sugar
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- 239000000284 extract Substances 0.000 title claims abstract description 114
- 240000000759 Lepidium meyenii Species 0.000 title claims abstract description 62
- 235000000421 Lepidium meyenii Nutrition 0.000 title claims abstract description 60
- 235000012902 lepidium meyenii Nutrition 0.000 title claims abstract description 60
- 238000005516 engineering process Methods 0.000 title abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 137
- 235000000346 sugar Nutrition 0.000 claims abstract description 30
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 239000011229 interlayer Substances 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 55
- 235000021551 crystal sugar Nutrition 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 29
- 238000001953 recrystallisation Methods 0.000 claims description 13
- 239000000469 ethanolic extract Substances 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 7
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 3
- 229920001542 oligosaccharide Polymers 0.000 abstract description 9
- 150000002482 oligosaccharides Chemical class 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000004615 ingredient Substances 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 90
- 238000002425 crystallisation Methods 0.000 description 15
- 230000008025 crystallization Effects 0.000 description 14
- -1 sulphur glycoside Chemical class 0.000 description 10
- 150000002016 disaccharides Chemical class 0.000 description 9
- 150000001336 alkenes Chemical class 0.000 description 8
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 6
- 150000001720 carbohydrates Chemical class 0.000 description 6
- 235000014633 carbohydrates Nutrition 0.000 description 6
- 150000004676 glycans Chemical class 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229920001282 polysaccharide Polymers 0.000 description 6
- 239000005017 polysaccharide Substances 0.000 description 6
- 150000004043 trisaccharides Chemical class 0.000 description 6
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 5
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 5
- 239000005864 Sulphur Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 229930182470 glycoside Natural products 0.000 description 4
- 238000002137 ultrasound extraction Methods 0.000 description 4
- 239000002826 coolant Substances 0.000 description 3
- 239000012809 cooling fluid Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002772 monosaccharides Chemical class 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 241000219193 Brassicaceae Species 0.000 description 2
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 229930182558 Sterol Natural products 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
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- 238000000926 separation method Methods 0.000 description 2
- 150000003432 sterols Chemical class 0.000 description 2
- 235000003702 sterols Nutrition 0.000 description 2
- 238000007445 Chromatographic isolation Methods 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- UNXHWFMMPAWVPI-UHFFFAOYSA-N Erythritol Natural products OCC(O)C(O)CO UNXHWFMMPAWVPI-UHFFFAOYSA-N 0.000 description 1
- 229930091371 Fructose Natural products 0.000 description 1
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 1
- 239000005715 Fructose Substances 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 241000801118 Lepidium Species 0.000 description 1
- 208000008589 Obesity Diseases 0.000 description 1
- 208000034189 Sclerosis Diseases 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000003262 anti-osteoporosis Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 1
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- VDTNNGKXZGSZIP-UHFFFAOYSA-N carbutamide Chemical compound CCCCNC(=O)NS(=O)(=O)C1=CC=C(N)C=C1 VDTNNGKXZGSZIP-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001212 derivatisation Methods 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 235000013325 dietary fiber Nutrition 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000002124 endocrine Effects 0.000 description 1
- UNXHWFMMPAWVPI-ZXZARUISSA-N erythritol Chemical compound OC[C@H](O)[C@H](O)CO UNXHWFMMPAWVPI-ZXZARUISSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000004383 glucosinolate group Chemical group 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000003908 liver function Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000020824 obesity Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000019100 sperm motility Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Tea And Coffee (AREA)
- Saccharide Compounds (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to a technology for crystallizing and purifying oligosaccharide of a maca extract. The technology comprises the following steps: (1) concentrating the maca extract in a vacuum concentrator and recovering an extracting agent so as to obtain a concentrated extract; (2) dissolving the concentrated extract in edible ethanol so as to obtain a maca extract ethanol solution;(3) transferring the maca extract ethanol solution in an interlayer crystallizing tank; (4) stirring the maca extract ethanol solution at -5-10 DEG C and applying ultrasonic wave; (5) keeping the maca extract ethanol solution for 6-24h and filtering so as to obtain crystallized sugar and an ethanol solution (1); (6) dissolving the crystallized sugar in edible ethanol, and repeating the steps (3)-(5) twice so as to obtain recrystallized sugar, an ethanol solution (2) and an ethanol solution (3); and (7) mixing the ethanol solutions (1), (2) and (3), and concentrating so as to obtain a sugar-removed maca extract. The sugar-removing technology disclosed by the invention is low in energy consumption, high in product purity and good in safety, and capable of protecting functional ingredients from losing.
Description
Technical field
The present invention relates to a kind of method except sugar, particularly relate to a kind of technique of Maca extract crystallization purifying oligosaccharides, belong to a kind of Maca extract concentration technique.
Background technology
Agate coffee (Maca), it is the block root of the annual or 2 years raw plant Macas (L.meyenii Walp.) of Cruciferae (Cruciferae) separate row Vegetable spp (Lepidium), research shows, containing abundant vitamin, mineral matter, amino acid and dietary fiber in agate coffee, and containing the abundant function composition such as macamide, agate coffee alkene, glucosinolate, polysaccharide, sterol, there is develop immunitypty, dispelling fatigue, raising sperm motility, treatment rheumatism, regulate endocrine, improve memory, treatment climacteric metancholia, anti-osteoporosis, the function such as anticancer.
Monose is generally polyhydroxy aldehyde containing 3-6 carbon atom or polyhydroxyketone, disaccharide is that bimolecular monose is formed by glycosidic bond, polysaccharide is formed by multiple monosaccharide molecule condensation, dehydration, be molecule mechanism complexity and huge glucide, oligosaccharide is generally the sugar that 2 ~ 10 monose are connected to form with glycosidic bond, and monosaccharide and disaccharide or oligosaccharide are generally all called oligosaccharides.Monose and disaccharide can provide heat energy to human body; also be the important substance forming tissue and protection liver function; but Excess free enthalpy can cause the diseases such as obesity, artery sclerosis, hypertension, diabetes and carious tooth, oligosaccharide and polysaccharide generally have very strong antiviral activity, antitumor activity, anti-inflammatory activity, antioxidation activity and immunity moderation and fall three high effects.
Some crystal sugar techniques are also had now to may be used for extract except sugar, be in the Chinese patent of CN103060482A as authorized publication number, disclose a kind of technique of production of corn starch crystal diabetin, this technology utilization glucose obtains fructose, and obtain the higher aqueous solution of purity by chromatographic isolation, then time row vacuum evaporating crystalization.And for example publication number is in the Chinese patent of CN102992957A, discloses a kind of dilution crystallization method of antierythrite, and crystallization is carried out in the handy dissolved agent of the method, can obtain the sugar alcohol product that quality is higher.For another example Authorization Notice No. is in the Chinese patent of CN10253453B, discloses a kind of method improving crystallization yield of xylose, and the mode of the handy gradient cooling of the method, improves crystallization yield.
Agate coffee is external advantitious plant, is approved as new resource food in 2011 by the Ministry of Public Health, and up to the present domestic research is less, does not have special polysaccharide purification method.Above-mentioned and other existing carbohydrate crystallization purifications, also exists or technique is more complicated, cost is higher, or needs to add the dissolved agent that cannot eat, the reasons such as poor stability, and is not exclusively applicable to agate coffee except sugared technique.
In sum, also do not have a kind of simple to operate at present, cost is low, device simple, and energy consumption is low, and purity is high, and security is good, can ensure that the loss-free Maca extract of effective component is except sugared purification process.
Summary of the invention
The object of the invention is to overcome above shortcomings in prior art, and provide a kind of simple to operate, cost is low, device simple, and energy consumption is low, and purity is high, and security is good, can ensure that the loss-free Maca extract of effective component is except sugared technique.
The present invention's adopted technical scheme that solves the problem is: this Maca extract is except the feature of sugared technique: this technique comprises the steps:
(1) be placed in vacuum concentrator by agate coffee extract, 35 ~ 50 DEG C of temperature, under the pressure of 5 ~ 12Kpa, concentration and recovery extractant, obtains concentrated extract;
(2) concentrated extract that step (1) obtains is dissolved in edible ethanol, the weight of edible ethanol used is 15 ~ 25 times of concentrated extract weight, stir, in faint yellow clear solution, this solution is placed in vacuum rotary evaporator, 35 DEG C of temperature, under the pressure of 12Kpa, be concentrated into 3 ~ 10 times that volume is concentrated extract, obtain Maca extract ethanolic solution;
(3) the Maca extract ethanolic solution that step (2) obtains is placed in interlayer crystallizing tank, stand at low temperature 24 ~ 48 hours;
(4) by leave standstill after Maca extract ethanolic solution be placed in-5 ~ 10 DEG C of temperature under, at the uniform velocity stir 30min with the speed of 60 turns/min, while stirring, to Maca extract ethanolic solution apply ultrasonic wave;
(5) the Maca extract ethanolic solution in step (4) is left standstill 6 ~ 24 hours, filter, obtain crystal sugar and ethanolic solution 1.;
(6) crystal sugar is dissolved in edible ethanol, the weight of edible ethanol used be the 7-13 of crystal sugar weight doubly, repeat step (3) ~ (5) twice, obtain recrystallization sugar, ethanolic solution 2. with ethanolic solution 3.;
(7) mixed ethanol solution 1., ethanolic solution 2. with ethanolic solution 3., and be placed in vacuum concentrator concentrate, obtain except sugar Maca extract medicinal extract.
Make the present invention while except sugar thus, effectively can guarantee that the functional components such as agate coffee alkene, macamide and the sulphur glycoside contained in Maca extract do not lose, whole technical process simple to operate, cost is low, device simple, and energy consumption is low, purity is high, and security is good.
As preferably, the agate coffee extract in step of the present invention (1) is agate coffee ethanol extract or agate coffee ethanol water mixed extract.
As preferably, in step of the present invention (2), be concentrated into 3 ~ 5 times that volume is concentrated extract.
As preferably, in step of the present invention (3), the temperature that Maca extract ethanolic solution leaves standstill in interlayer crystallizing tank is 5 ~ 15 DEG C.
As preferably, in step of the present invention (4), supersonic frequency is between 20 ~ 50kHz.
The present invention compared with prior art, has the following advantages and effect: (1) whole technique only adopts edible ethanol to be solvent, and security is high.(2) adopt single interlayer crystallizing tank as crystallization except sugared container, be beneficial to solution cooling, equipment is simple, and cost is low, processing ease.(3) adopt ultrasonic wave to accelerate carbohydrate crystallization nucleation in Maca extract, save time.(4), while nucleation, adopt agitating mode, avoid nucleus to be bonded on crystallization tank skin, affect crystal and be separated with solution.(5) purity is high, active principle free of losses, and after three recrystallizations, the purity of the agate coffee crystal sugar of acquisition can reach more than 99%, and the loss of agate coffee effective ingredient is lower than less than 0.5%; Inventor's research shows, containing mass percent in agate coffee block root is the polysaccharide of 3 ~ 8% and the oligosaccharides of 17 ~ 24%, the present invention is in order to by oligosaccharides purifies and separates in Maca extract, liquid chromatographic detection result and molecular weight analyse result show, agate coffee crystal sugar mainly glucosyl group monosaccharide and disaccharide and trisaccharide, wherein based on maltose, ethanol can be slightly soluble in.In Maca extract except containing the oligosaccharides of 1 ~ 3 monose, also containing functional components such as agate coffee alkene, macamide and sulphur glycosides, the present invention mainly in order to remove glucosyl group monosaccharide and disaccharide in Maca extract and trisaccharide, and effectively ensure that the functional components such as agate coffee alkene class, macamide class, agate coffee sulphur glycoside, agate coffee sterols, maca polysaccharide class do not lose while except sugar.
Accompanying drawing explanation
Fig. 1 is that embodiment of the present invention monose derivatization standard sample HPLC schemes, and wherein, 12 ~ 13min peak is glucose.
Fig. 2 is embodiment of the present invention Maca extract crystal sugar simple monosaccharide composition HPLC figure.
Detailed description of the invention
Below in conjunction with accompanying drawing, also by embodiment, the present invention is described in further detail, and following examples are explanation of the invention and the present invention is not limited to following examples.
Embodiment 1.
Maca extract in the present embodiment is removed sugared technique and is comprised the steps.
(1) by agate coffee extract in vacuum concentrator, in 35 ~ 50 DEG C of temperature, under the pressure of 5 ~ 12Kpa, concentration and recovery extractant.Agate coffee extract in the present invention can be ethanol extract or the water alcohol mixed extract of agate coffee, and the water alcohol mixed extract of agate coffee refers to the extract obtained with ethanol water extraction agate coffee.By agate coffee extract under the environment of low temperature, low pressure, reclaim extractant, obtain concentrated extract, containing agate coffee alkene, macamide and sulphur glycoside function composition in this concentrated extract, and a large amount of sugared parts.
(2) concentrated extract that step (1) obtains is dissolved in edible ethanol, the weight of edible ethanol used is the weight of the concentrated extract of 15 ~ 25 times, stir, in faint yellow clear solution, again in vacuum rotary evaporator, 35 DEG C of temperature, under the pressure of 12Kpa, by volume concentration to 3 ~ 10 times of concentrated extract volume.Concentrated extract is dissolved in pure edible ethanol, can adopt if desired and stir assist in dissolving, ultrasonic wave added dissolves, concentrated extract is dissolved in ethanol completely, Maca extract ethanolic solution is generally in light yellow, now containing macamide, agate coffee alkene, sulphur glycosides compound and carbohydrate in solution, is the unsaturated solution of carbohydrate.By the carbohydrate unsaturated solution of Maca extract in 35 DEG C of temperature, the vacuum under pressure of 12Kpa is concentrated into 3 ~ 10 times that volume is concentrated extract, forms the supersaturated solution of carbohydrate.
(3) by the Maca extract ethanolic solution that step (2) obtains, interlayer crystallizing tank is placed in, stand at low temperature 24 ~ 48 hours; Under normal circumstances, poured in interlayer crystallizing tank by Maca extract ethanolic solution, interlayer leads to cooling fluid, and coolant temperature, between 5 ~ 15 DEG C, leaves standstill 24 ~ 48 hours, supersaturation sugar juice is down to completely temperature required, whole solution system, temperature stabilization.
(4) by the agate coffee ethanolic solution that left standstill at-5 ~ 10 DEG C of temperature, at the uniform velocity 30min is stirred with the speed of 60 turns/min, while stirring, 20 ~ 50kHz frequency ultrasonic wave is applied to solution and promotes that the nucleus of sugar produces, best supersonic frequency is 25 ~ 35kHz, nucleus can be made within 5min to be formed rapidly and basic growing the grain terminates, the stirring at low speed while of applying hyperacoustic to solution, be chamber wall formed a large amount of nucleus to prevent and grow up into crystal, cause next step solution and crystal separation difficulty.Adopt high-speed stirred also can promote that supersaturation agate coffee ethanol sugar juice nucleus is formed, but mixing speed will at 800 turns/more than min, this easily realizes in laboratory conditions, industrialized main equipment, so high rotating speed, cause the high shear force between blade and solution, be easy to promote that nucleus is formed, but also very easily cause the temperature of solution to rise, hinder the formation of nucleus on the contrary, the present invention utilizes ultrasonic promotion nucleus to be formed, and stirring at low speed prevents wall crystallization, nucleus can be formed very soon, can prevent again temperature from rising.
(5) solution left standstill step (4) obtained 6 ~ 24 hours, filters, and is separated and obtains crystal sugar and ethanolic solution 1.; Under normal circumstances, solution after the nucleus that step (4) obtains is formed is at 5 ~ 15 DEG C of temperature, leave standstill growing the grain 6 ~ 24 hours, crystal is fully formed, by the valve open bottom crystallizing tank, filter, be separated the agate coffee ethanol extract obtaining crystal sugar and desugar, namely crystal sugar and ethanolic solution are 1..
(6) crystal sugar in step (5) is dissolved in the edible ethanol of 10 times of crystal sugar weight again, repeats step (3) ~ (5) twice, obtain recrystallization sugar, ethanolic solution 2. with ethanolic solution 3..The nucleus of partially crystallizable sugar may be the effective ingredient particle of agate coffee, and also part effective ingredient can be wrapped in the inside in sugared crystallization process, redissolve recrystallization process twice, can obtain the crystal sugar that purity reaches 99%.
(7) ethanolic solution that obtains of blend step (5) and (6) 1., ethanolic solution 2. with ethanolic solution 3., concentrated in vacuum concentrator, obtain the Maca extract medicinal extract except sugar.Usually please see down, by three Crystallization Separation to agate coffee ethanolic solution in Vacuum Concentration container, 35 DEG C of temperature, under the pressure of 12Kpa, reclaim ethanol completely, obtain the Maca extract medicinal extract except sugar.
Shown by the liquid chromatographic detection result of Fig. 1 and Fig. 2 and molecular weight analyse result, agate coffee crystal sugar mainly glucosyl group monosaccharide and disaccharide and trisaccharide, wherein based on maltose, can be slightly soluble in ethanol.
Embodiment 2.
Maca extract in the present embodiment is removed sugared technique and is comprised the steps.
(1) get 100Kg agate coffee dry sliced, be crushed to 200 orders, pour in ultrasonic extraction still, the percent by volume adding 500Kg is the edible ethanol of 80%, ultrasonic extraction 3 times, merges extract, obtains 1600Kg agate coffee ethanol water mixed extract altogether.
(2) agate coffee ethanol water mixed extract is poured in continous way Rotary Evaporators, 35 DEG C of temperature, under the vacuum of 10Kpa pressure, concentration and recovery ethanol, then in 40 DEG C of temperature, under the vacuum of 8Kpa pressure, concentration and recovery water, obtains 22Kg and carries concentrated extract.
(3) concentrated extract is dissolved in the edible ethanol of 440Kg, stirs, in faint yellow clear solution, then the edible ethanol solution dissolved is placed in continuous vacuum Rotary Evaporators, 35 DEG C of temperature, under the pressure of 12Kpa, volume concentration to 120 liter.
(4) the 120L agate coffee ethanolic solution in step (3) is placed in interlayer crystallizing tank, crystallizing tank interlayer leads to 10 DEG C of cooling fluids, stand at low temperature 24 hours.
(5) crystallizing tank coolant temperature is adjusted to-5 DEG C of temperature, after stable, at the uniform velocity stirs agate coffee ethanolic solution 30min with the speed of 60 turns/min, while stirring, solution is applied to the ultrasonic wave of 35KHz, in solution, form fine crystalline body.
(6) by the solution left standstill 12 hours of ultrasonic rear acquisition, make crystal sugar crystallization complete, filter, be separated and obtain crystal sugar 20Kg and ethanolic solution 1. 100L.
(7) crystal sugar obtained in step (6) is dissolved in the edible ethanol of 200L again, repeat step (4) ~ (6) twice, obtain the sugared 19.9Kg of recrystallization, ethanolic solution 2. with ethanolic solution 3., 2. ethanolic solution adds up to 400L with ethanolic solution volume 3..
(8) ethanolic solution that obtains of blend step (6) and (7) 1., 3. 2. ethanolic solution add up to 500L with ethanolic solution, in continous way Rotary Evaporators, 35 DEG C of temperature, under the pressure of 12Kpa, Vacuum Concentration reclaims ethanol, obtain except sugar Maca extract medicinal extract 2Kg, in medicinal extract macamide and agate coffee alkene content comparatively do not eliminate sugar time improve 10 times.
Shown by the liquid chromatographic detection result of Fig. 1 and Fig. 2 and molecular weight analyse result, agate coffee crystal sugar mainly glucosyl group monosaccharide and disaccharide and trisaccharide, wherein based on maltose, can be slightly soluble in ethanol.
Embodiment 3.
Maca extract in the present embodiment is removed sugared technique and is comprised the steps.
(1) get 500Kg agate coffee xeraphium, pour in ultrasonic extraction still, add the edible ethanol of 3000Kg, ultrasonic extraction 3 times, merge extract, obtain 9500Kg agate coffee ethanol extract altogether.
(2) agate coffee ethanol extract is poured in continous way Rotary Evaporators, 35 DEG C of temperature, under the vacuum of 10Kpa pressure, concentration and recovery ethanol, volume concentration to 1000 liter.
(3) 1000L agate coffee ethanolic solution is placed in interlayer crystallizing tank, crystallizing tank interlayer leads to 5 DEG C of cooling fluids, stand at low temperature 48 hours.
(4) crystallizing tank coolant temperature is adjusted to 0 DEG C of temperature, after stable, at the uniform velocity stirs agate coffee ethanolic solution 30min with the speed of 60 turns/min, while stirring, solution is applied to the ultrasonic wave of 25KHz, in solution, form fine crystalline body, and the basic nodeless mesh of crystallization tank skin.
(5) by the solution left standstill 24 hours of ultrasonic rear acquisition, make crystal sugar crystallization complete, filter, be separated and obtain crystal sugar 95Kg and ethanolic solution 900L.
(6) crystal sugar obtained in step (5) is dissolved in the edible ethanol of 1000L again, repeats step (3) ~ (5) twice, obtain recrystallization sugared 94Kg and ethanolic solution 2000L.
(7) the ethanolic solution 2900L that obtains of blend step (5) and (6), in continous way Rotary Evaporators, 35 DEG C of temperature, under the pressure of 12Kpa, Vacuum Concentration reclaims ethanol, obtain except sugar Maca extract medicinal extract 7.5Kg, in medicinal extract macamide and agate coffee alkene content comparatively do not eliminate sugar time improve 12 times.
Shown by the liquid chromatographic detection result of Fig. 1 and Fig. 2 and molecular weight analyse result, agate coffee crystal sugar mainly glucosyl group monosaccharide and disaccharide and trisaccharide, wherein based on maltose, can be slightly soluble in ethanol.
Embodiment 4.
Maca extract in the present embodiment is removed sugared technique and is comprised the steps.
(1) be placed in vacuum concentrator by agate coffee extract, 35 ~ 50 DEG C of temperature, under the pressure of 5 ~ 12Kpa, concentration and recovery extractant, obtains concentrated extract.Agate coffee extract in step (1) can be agate coffee ethanol extract or agate coffee ethanol water mixed extract.
(2) concentrated extract that step (1) obtains is dissolved in edible ethanol, the weight of edible ethanol used is 15 ~ 25 times of concentrated extract weight, stir, in faint yellow clear solution, this solution is placed in vacuum rotary evaporator, 35 DEG C of temperature, under the pressure of 12Kpa, be concentrated into 3 ~ 10 times that volume is concentrated extract, obtain Maca extract ethanolic solution.The present invention can be concentrated into 3 ~ 5 times that volume is concentrated extract.
(3) the Maca extract ethanolic solution that step (2) obtains is placed in interlayer crystallizing tank, stand at low temperature 24 ~ 48 hours.The temperature that Maca extract ethanolic solution leaves standstill in interlayer crystallizing tank can be 5 ~ 15 DEG C.
(4) by leave standstill after Maca extract ethanolic solution be placed in-5 ~ 10 DEG C of temperature under, at the uniform velocity stir 30min with the speed of 60 turns/min, while stirring, to Maca extract ethanolic solution apply ultrasonic wave.Supersonic frequency can between 20 ~ 50kHz.
(5) the Maca extract ethanolic solution in step (4) is left standstill 6 ~ 24 hours, filter, obtain crystal sugar and ethanolic solution 1..
(6) be dissolved in edible ethanol by crystal sugar, obtain crystal sugar ethanolic solution, the weight of edible ethanol used is 7-13 times of crystal sugar weight.
(7) the crystal sugar ethanolic solution that step (6) obtains is placed in interlayer crystallizing tank, stand at low temperature 24 ~ 48 hours.The temperature that crystal sugar ethanolic solution leaves standstill in interlayer crystallizing tank can be 5 ~ 15 DEG C.
(8) by leave standstill after crystal sugar ethanolic solution be placed in-5 ~ 10 DEG C of temperature under, at the uniform velocity stir 30min with the speed of 60 turns/min, while stirring, to crystal sugar ethanolic solution apply ultrasonic wave.Supersonic frequency can between 20 ~ 50kHz.
(9) by the crystal sugar ethanolic solution in step (8) leave standstill 6 ~ 24 hours, filter, obtain recrystallization sugar 1. with ethanolic solution 2..
(10) 1. recrystallization sugar is dissolved in edible ethanol, obtains the sugared ethanolic solution that is recrystallized, the weight of edible ethanol used attach most importance to crystal sugar weight 7-13 doubly.
(11) recrystallization sugar ethanolic solution step (10) obtained is placed in interlayer crystallizing tank, stand at low temperature 24 ~ 48 hours.The temperature that the sugared ethanolic solution that is recrystallized leaves standstill in interlayer crystallizing tank can be 5 ~ 15 DEG C.
(12), under by the recrystallization sugar after leaving standstill, ethanolic solution is placed in-5 ~ 10 DEG C of temperature, at the uniform velocity stir 30min with the speed of 60 turns/min, while stirring, counterweight crystal sugar ethanolic solution applies ultrasonic wave.Supersonic frequency can between 20 ~ 50kHz.
(13) by step (12) recrystallization sugar ethanolic solution leave standstill 6 ~ 24 hours, filter, obtain recrystallization sugar 2. with ethanolic solution 3..
(14) mixed ethanol solution 1., ethanolic solution 2. with ethanolic solution 3., and be placed in vacuum concentrator concentrate, obtain except sugar Maca extract medicinal extract.
Shown by the liquid chromatographic detection result of Fig. 1 and Fig. 2 and molecular weight analyse result, agate coffee crystal sugar mainly glucosyl group monosaccharide and disaccharide and trisaccharide, wherein based on maltose, can be slightly soluble in ethanol.
Although the present invention with embodiment openly as above; but it is also not used to limit protection scope of the present invention; any technical staff being familiar with this technology, not departing from the change and retouching done in the spirit and scope of the present invention, all should belong to protection scope of the present invention.
Claims (5)
1. Maca extract is except a sugared technique, it is characterized in that: this technique comprises the steps:
(1) be placed in vacuum concentrator by agate coffee extract, 35 ~ 50 DEG C of temperature, under the pressure of 5 ~ 12Kpa, concentration and recovery extractant, obtains concentrated extract;
(2) concentrated extract that step (1) obtains is dissolved in edible ethanol, the weight of edible ethanol used is 15 ~ 25 times of concentrated extract weight, stir, in faint yellow clear solution, this solution is placed in vacuum rotary evaporator, 35 DEG C of temperature, under the pressure of 12Kpa, be concentrated into 3 ~ 10 times that volume is concentrated extract, obtain Maca extract ethanolic solution;
(3) the Maca extract ethanolic solution that step (2) obtains is placed in interlayer crystallizing tank, stand at low temperature 24 ~ 48 hours;
(4) by leave standstill after Maca extract ethanolic solution be placed in-5 ~ 10 DEG C of temperature under, at the uniform velocity stir 30min with the speed of 60 turns/min, while stirring, to Maca extract ethanolic solution apply ultrasonic wave;
(5) the Maca extract ethanolic solution in step (4) is left standstill 6 ~ 24 hours, filter, obtain crystal sugar and ethanolic solution 1.;
(6) crystal sugar is dissolved in edible ethanol, the weight of edible ethanol used be the 7-13 of crystal sugar weight doubly, repeat step (3) ~ (5) twice, obtain recrystallization sugar, ethanolic solution 2. with ethanolic solution 3.;
(7) mixed ethanol solution 1., ethanolic solution 2. with ethanolic solution 3., and be placed in vacuum concentrator concentrate, obtain except sugar Maca extract medicinal extract.
2. Maca extract according to claim 1 is except sugared technique, it is characterized in that: the agate coffee extract in described step (1) is agate coffee ethanol extract or agate coffee ethanol water mixed extract.
3. Maca extract according to claim 1 is except sugared technique, it is characterized in that: in described step (2), is concentrated into 3 ~ 5 times that volume is concentrated extract.
4. Maca extract according to claim 1 is except sugared technique, it is characterized in that: in described step (3), and the temperature that Maca extract ethanolic solution leaves standstill in interlayer crystallizing tank is 5 ~ 15 DEG C.
5. Maca extract according to claim 1 is except sugared technique, it is characterized in that: in described step (4), supersonic frequency is between 20 ~ 50kHz.
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| CN107446789A (en) * | 2017-07-27 | 2017-12-08 | 东华大学 | A kind of method that sugar content in liqueur beverage is reduced using the crystallizing process under low temperature |
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