CN104207134A - Production method of maca extracts - Google Patents
Production method of maca extracts Download PDFInfo
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- CN104207134A CN104207134A CN201410532870.3A CN201410532870A CN104207134A CN 104207134 A CN104207134 A CN 104207134A CN 201410532870 A CN201410532870 A CN 201410532870A CN 104207134 A CN104207134 A CN 104207134A
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- agate coffee
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- 239000000284 extract Substances 0.000 title claims abstract description 142
- 240000000759 Lepidium meyenii Species 0.000 title abstract description 11
- 235000000421 Lepidium meyenii Nutrition 0.000 title abstract description 9
- 235000012902 lepidium meyenii Nutrition 0.000 title abstract description 9
- 238000004519 manufacturing process Methods 0.000 title abstract 4
- 238000000605 extraction Methods 0.000 claims abstract description 61
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 56
- 239000007787 solid Substances 0.000 claims abstract description 53
- 239000012141 concentrate Substances 0.000 claims abstract description 51
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 238000000926 separation method Methods 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 140
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 139
- 238000003756 stirring Methods 0.000 claims description 31
- 125000004383 glucosinolate group Chemical group 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 25
- 241000219780 Pueraria Species 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 23
- 229920001282 polysaccharide Polymers 0.000 claims description 22
- 239000005017 polysaccharide Substances 0.000 claims description 22
- 150000001336 alkenes Chemical class 0.000 claims description 20
- 150000001408 amides Chemical class 0.000 claims description 20
- 150000004676 glycans Chemical class 0.000 claims description 20
- 229930182558 Sterol Natural products 0.000 claims description 15
- 150000003432 sterols Chemical class 0.000 claims description 15
- 235000003702 sterols Nutrition 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000002425 crystallisation Methods 0.000 claims description 10
- 230000008025 crystallization Effects 0.000 claims description 10
- 239000011229 interlayer Substances 0.000 claims description 8
- 235000000346 sugar Nutrition 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000003814 drug Substances 0.000 claims description 4
- 235000013305 food Nutrition 0.000 claims description 4
- 230000036541 health Effects 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 7
- 238000000034 method Methods 0.000 description 20
- 229920002472 Starch Polymers 0.000 description 17
- 239000008107 starch Substances 0.000 description 17
- 235000019698 starch Nutrition 0.000 description 17
- 239000008187 granular material Substances 0.000 description 14
- 230000008569 process Effects 0.000 description 9
- -1 Saccharide compound Chemical class 0.000 description 8
- 238000011084 recovery Methods 0.000 description 8
- 239000004615 ingredient Substances 0.000 description 7
- 238000002386 leaching Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 230000006870 function Effects 0.000 description 5
- 239000004480 active ingredient Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 229920001542 oligosaccharide Polymers 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 239000003818 cinder Substances 0.000 description 3
- 230000004087 circulation Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000003809 water extraction Methods 0.000 description 3
- 241000219193 Brassicaceae Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000469 ethanolic extract Substances 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 230000002779 inactivation Effects 0.000 description 2
- 238000002525 ultrasonication Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000801118 Lepidium Species 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003262 anti-osteoporosis Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 235000021551 crystal sugar Nutrition 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000002124 endocrine Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012530 fluid Substances 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
- 238000000227 grinding Methods 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000019100 sperm motility Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/30—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
- A23L5/32—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation using phonon wave energy, e.g. sound or ultrasonic waves
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/31—Brassicaceae or Cruciferae (Mustard family), e.g. broccoli, cabbage or kohlrabi
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- 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
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Abstract
The invention relates to a production method of maca extracts. The production method comprises the following steps of step 1, slicing a maca root; step 2, performing crushing and ultrasonic extraction; step 3, releasing an upper layer of extraction solution and performing ultrasonic extraction; step 4, releasing an upper layer of extraction solution and performing ultrasonic extraction; step 5, performing squeezing separation to obtain an upper layer of extraction solution and extraction residues; step 6, combining the upper layers of extraction solutions in the step 3, the step 4 and the step 5 and performing centrifugal separation to obtain solids (1) and a clear solution (2); step 7, performing vacuum concentration on the clear solution (2) to obtain the concentrate (3); step 8, performing solid-liquid separation on the solids (1) to obtain an extracting solution and solids; step 9, performing solid-liquid separation on the solids to obtain an extracting solution and solids; step 10, combining the extracting solutions in the step 8 and the step 9 and performing vacuum concentration to obtain the extract concentrate (4); step 11, performing ultrasonic extraction on the extraction residues in the step 5 to obtain the extract concentrate (5); step 12, combining the concentrate in the step 7, the step 10 and the step 11 to obtain the maca extracts. According to the production method of the maca extracts, the activity loss is not produced and the extracts are rich.
Description
Technical field
The present invention relates to a kind of preparation method of agate coffee extract, belong to the method for several functions active ingredient in a kind of simple extraction agate coffee, extract can be used in food, health product and medicine.
Background technology
Agate coffee (Maca), be Cruciferae (Cruciferae) separate row Vegetable spp (Lepidium) annual or 2 years raw plant Maca (L.meyenii Walp.) piece root, research shows, agate coffee have strengthen immunity, eliminate tired, improve sperm motility, treatment rheumatism, regulate endocrine, improve memory, treatment climacteric metancholia, anti-osteoporosis, the function such as anticancer, its major function active material is agate coffee acid amides, agate coffee alkene, glucosinolate, sterol and polysaccharide etc.
Most of active materials in agate coffee are to sensitive, temperature can make its loss of activity, particularly agate coffee alkene, agate coffee acid amides and polysaccharide etc., and the temperature that surpasses 60 ℃ will exert an influence to its function, but the extraction temperature of glucosinolates is substantially all more than 80 ℃, and optimum temperature is 90 ℃ of left and right.So, in agate coffee extracting method, if extracted at low temperatures, can cause the functional component glucosinolates recovery rate in agate coffee low, if at high temperature extracted, can affect the activity of the function composition in agate coffee.
If open day is on 01 22nd, 2014, in the Chinese patent that publication number is CN103519180A, a kind of preparation method of agate coffee extract is disclosed, this preparation method comprises: the (1) preparation of agate coffee extract; (2) the pretreatment of agate coffee extract; (3) ceramic membrane filter; (4) Vacuum Concentration; (5) spraying is dry; Although the content of active ingredient glucosinolate is higher in the prepared extract of the method, concentrate need to be sprayed dry, and leaving air temp is controlled at 70-80 ℃, cause the active component in extract to destroy.And for example open day is on 04 17th, 2013, publication number is in the Chinese patent of CN103040896A, a kind of preparation method of agate coffee extract is disclosed, the pueraria root powder that this preparation method processes the enzyme that goes out is put into extractor, and the ethanol that the mass concentration that adds 7～9 times of amounts of pueraria root powder quality is 95%, soaks 1～3 hour, when being heated to fluid temperature and being 70～85 ℃, refluxing extraction 2～4 hours, separated a extract and recrement, the destruction that has caused active component in agate coffee.For another example open day is on December 26th, 2012, publication number is in the Chinese patent of CN102836196A, a kind of agate coffee extract and preparation method thereof is disclosed, this agate coffee method for preparing extractive comprises raw material processing, circulation extraction, purifying, concentrated and drying steps, be specially: A, raw material process: select without rotting, without going mouldy, without the agate coffee of the visible exogenous impurity of naked eyes, getting its dry root, to carry out fine powder broken, and grinding particle size is to pass through 60～100 mesh sieves; B, circulation are extracted: the raw material after pulverizing drops in extractor, add 45～55 ℃ of circulations of 50%～90 % alcoholic solution of 7～9 times of amounts of weight ratio to extract 2～5h, obtain extract; C, purifying: extract is put into settling tank natural sedimentation 6～10h, get supernatant and carry out vacuum filtration, and filtrate is centrifugal with the rotating speed of 10000～40000r/min with supercentrifuge; D, concentrated and dry: extracting centrifugal liquid at 40～55 ℃ of Vacuum Concentrations to relative density 1.0～1.3, at 40～55 ℃ after dry agate coffee extract, because the extraction temperature of the method is 45～55 ℃, so the glucosinolates recovery rate in agate coffee is low.
In sum, also do not have at present a kind of technique simple, extraction efficiency is high, active free of losses, the agate coffee method for preparing extractive that extract is abundant.
Summary of the invention
The object of the invention is to overcome above shortcomings in prior art, and provide a kind of technique simple, extraction efficiency is high, active free of losses, the preparation method of the agate coffee extract that extract is abundant.
The present invention addresses the above problem adopted technical scheme: the preparation method's of this agate coffee extract feature is: comprise the steps:
(1) by agate coffee piece undercut sheet, obtain agate coffee sheet, the moisture content of agate coffee sheet is 2～5%;
(2) agate coffee sheet is pulverized, obtain pueraria root powder, pueraria root powder is added in the ultrasonic extraction still of interlayer, add edible ethanol, the weight ratio of pueraria root powder and edible ethanol is 1:5～1:10 again, and low whipping speed is 60 revs/min, temperature is 5～40 ℃, frequency is 20～45KHz, under the condition that power is 1000～1700W, and ultrasonic extraction 1～2 hour;
(3) after the ultrasonic extraction of step (2) finishes, close stirring, within 30～90 second time, solution being extracted in upper strata emits, in leftover materials, add edible ethanol, the weight of the edible ethanol adding is 3-7 times of pueraria root powder weight, and low whipping speed is 60 revs/min, temperature is 5～40 ℃, frequency is 20～45KHz, under the condition that power is 1000～1700W, and ultrasonic extraction 1～2 hour;
(4) after the ultrasonic extraction of step (3) finishes, close stirring, within 30～90 second time, solution being extracted in upper strata emits, in leftover materials, add edible ethanol, the weight of the edible ethanol adding is 3-7 times of pueraria root powder weight, and low whipping speed is 60 revs/min, temperature is 5～40 ℃, frequency is 20～45KHz, under the condition that power is 1000～1700W, and ultrasonic extraction 1～2 hour;
(5) after the ultrasonic extraction of step (4) finishes, close stirring, pour material in still in solid-liquid separating machine expression separation, obtain upper strata and extract solution and extract residue;
(6) solution is extracted on combining step (3), (4) and (5) obtain upper strata, and solution is extracted in the upper strata of this merging joins in low-temperature and high-speed centrifuge, at 5～15 ℃ of temperature, centrifugation obtain solid content 1. with clear liquid 2.;
(7) by clear liquid 2. 35 ℃ of temperature, under 10KPa pressure, carry out Vacuum Concentration, reclaim edible ethanol and crystallization except sugar, obtain and extract concentrate 3., 3. this extraction concentrate comprises agate coffee alkene, agate coffee acid amides and sterol;
(8) 1. solid content is joined and stir in extraction still, adding volumn concentration is 75% edible ethanol, 1. solid content is 1:4～1:6 with the weight ratio of the volumn concentration edible ethanol that is 75%, at 90 ℃ of temperature, stir and extract 1 hour, standing 25 minutes, Separation of Solid and Liquid, obtained extract and solid content;
(9) to adding volumn concentration in the solid content of step (8), be 75% edible ethanol, the weight ratio of the edible ethanol that solid content and volumn concentration are 75% is 1:4～1:6, at 90 ℃ of temperature, stir and extract 1 hour, standing 25 minutes, Separation of Solid and Liquid, obtained extract and solid content;
(10) extract that combining step (8) and (9) obtain, 45 ℃ of temperature, 10KPa vacuum under pressure is concentrated, obtains and extracts concentrate 4., and 4. this extraction concentrate comprises glucosinolate;
(11) to the pure water that adds 5 times of volumes in the extraction residue of step (5), at 60 ℃, ultrasonic extraction three times, merge extract, Vacuum Concentration is removed 90% moisture content, then adds the edible ethanol that the volumn concentration of 3 times of volumes is 95%, standing 5 hours, 5. collecting precipitation, to extract concentrate, and this extraction concentrate mainly comprises the thick polysaccharide of agate coffee in 5.;
(12) the extraction concentrate of the extraction concentrate of the extraction concentrate in combining step (7) 3., in step (10) 4. and in step (11) 5., obtains agate coffee extract.
In ultrasonic leaching process, adopt the ultrasonic temperature of 5～40 ℃, the supersonic frequency of 20～45KHz, the ultrasonic power of 1000～1700W, powerful ultrasonic, can produce stronger cavitation demolition effect, also make starch granules more easily be precipitated, compared with low temperature, guaranteed that extract can excessively not heat up because of ultrasonication, make the easier strippings of effective ingredient such as agate coffee alkene, agate coffee acid amides, polysaccharide and sterol, at lower temperature, extract more thoroughly, so both guaranteed recovery rate, make again the active ingredient can Yin Gaowen and inactivation.
Saccharide compound in agate coffee material, except the non-functional long-chain saccharide compounds such as starch, cellulose and functional polysaccharide compounds, the oligosaccharide compound that also has 1～3 glucosyl group of part to form, its content accounts for 17～23% of agate coffee, if adopting water alcohol extracting follows the example of, can cause polysaccharide and glucosyl group oligosaccharides in extract all can be suggested, have a strong impact on the crystallization purifying technique of follow-up glucosyl group oligosaccharides.
Agate coffee is in ultrasonic leaching process, the starch granules absorption that effective ingredient glucosinolate compounds is more easily precipitated, and in starch granules, substantially do not contain agate coffee alkene, the compositions such as agate coffee acid amides and polysaccharide, in 30～90 seconds after ultrasonic extraction finishes, solution being extracted in upper strata emits, starch granules is flowed out together with extract, at next step, carry out separation, undermost solid content is added to edible ethanol again to be repeated to extract, technique is ingenious, extraction efficiency is high, under cryogenic conditions, effective ingredient glucosinolate compounds is extracted with the form being adsorbed on starch granules, both protected agate coffee alkene, agate coffee acid amides, the activity of the effective ingredient such as polysaccharide and sterol, reached again the object of extracting effective ingredient glucosinolate compounds, if overcome in agate coffee leaching process and will extract glucosinolate compounds, can only destroy agate coffee alkene, the technology prejudice of agate coffee acid amides and sterol isoreactivity, can be by the agate coffee alkene in agate coffee, agate coffee acid amides, polysaccharide and sterol first extract, again glucosinolate compounds is extracted, from residue, maca polysaccharide is extracted again, extract enriches complete.
The present invention pays parameter and the reagent that has used science after creative work, first adopt ultrasonic low temperature alcohol extracting, obtain agate coffee alkene, agate coffee acid amides and sterol, extract is removed crystal sugar, adopt again glucosinolate compounds in supersonic high temperature water alcohol extracting starch, water extraction maca polysaccharide from extract residue again, extract for three times and obtain agate coffee alkene, agate coffee acid amides, sterol, glucosinolate and polysaccharide, extract enriches complete, the extraction reagent difference that three steps are used, high recovery rate and purification efficiency have been guaranteed, the extraction temperature difference that three steps are used, both guaranteed recovery rate, prevented again the sex change of temperature-sensitive thing.
As preferably, in step of the present invention (2), agate coffee sheet is crushed to 300～500 object fineness.In ultrasonic leaching process, the particle of this yardstick, is easy to starch granules in pueraria root powder to separate out, and makes glucosinolate compounds in material more easily by starch adsorption.
As preferably, in step of the present invention (2) and step (3), the power of ultrasonic extraction is 1500W～1700W, and in step (4), the power of ultrasonic extraction is 1000-1200W.Step (2) and step (3) adopt high-power high sound pressure ultrasonic, can produce large cavitation bubble, and cavitation intensity is large, and the fragmentation that is beneficial to material is extracted; During step (4) adopts, the low acoustic pressure of power is ultrasonic, can produce little and fine and closely woven cavitation bubble, and cavitation intensity is smaller, but is beneficial to the extraction of active principle in small material.
As preferably, in step of the present invention (2) and step (3), the frequency of ultrasonic extraction is 20-25KHz, and in step (4), the frequency of ultrasonic extraction is 35-45KHz.Step (2) and step (3) adopt low frequency ultrasound, can produce large cavitation bubble, and the ratio of bubble full-size and initial size is large, and cavitation intensity is large, are conducive to the broken of initial material and extract; Step (4) adopts high frequency ultrasound, produces fine and closely woven cavitation bubble, and the ratio of bubble full-size and initial size is little, and number of bubbles is many during than low frequency, is of value to the extraction of active principle in small particles material.
As preferably, in step of the present invention (8), 1. solid content is 1:5 with the weight ratio of the volumn concentration edible ethanol that is 75%.
As preferably, in step of the present invention (9), the weight ratio of the edible ethanol that solid content and volumn concentration are 75% is 1:5.
An agate coffee extract, its feature is: adopt above-mentioned preparation method to make.
An application for agate coffee extract, its feature is: this agate coffee extract application on food.
An application for agate coffee extract, its feature is: this agate coffee extract application on health product.
An application for agate coffee extract, its feature is: this agate coffee extract application on medicine.
The present invention compared with prior art, has the following advantages and effect:
(1) extraction efficiency is high, adopts fine granular materials two infra-low frequency high-energy ultrasonics to extract, the ultrasonic extraction of energy in a high frequency, and in agate coffee, the extraction efficiency of characteristic secondary metabolites agate coffee acid amides and agate coffee alkene can reach more than 95%.
(2) extract is abundant, first adopt straight alcohol to extract, obtain extracting section thing, adopt again glucosinolate compounds in ultrasonic water alcohol extracting starch, to residue, adopt ultrasonic water extraction to obtain polysaccharide compound again, three extractions can obtain agate coffee alkene, agate coffee acid amides, polysaccharide, sterol and glucosinolate, and extract enriches complete.
(3) extraction temperature is suitable, the ultrasonic alcohol extracting of the first step, adopt 40 ℃ with interior extraction temperature, avoid the temperature-sensitive sex change of extract, second step and the 3rd step adopt 90 ℃ at water alcohol extracting and 60 ℃ of water extractions, guaranteed high recovery rate, the extraction temperature that three steps are different, guarantee recovery rate, prevented again the sex change of temperature-sensitive thing.
(4) extracting method safety, the present invention's extractant used is independent edible ethanol, edible ethanol water intermixture and pure water, extractant safety, noresidue after Vacuum Concentration.
The specific embodiment
Below 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.
In the present embodiment, the preparation method of agate coffee extract comprises the steps.
(1) select ripe agate coffee piece root, with drinking water, clean up, section is dried to moisture content 4% at 45 ℃ of temperature.
(2) dried agate coffee sheet is crushed to 500 orders, the pueraria root powder 100Kg crushing is added in the ultrasonic extraction still of interlayer, add 700Kg edible ethanol, under the mixing speed of 60 revs/min, at 40 ℃ of temperature, 22KHz frequency, under 1500W power, ultrasonic extraction 1 hour.
(3) after ultrasonic end, close stirring, within 60 second time, solution is extracted in upper strata and emit, in leftover materials, add 500Kg edible ethanol, in 22KHz frequency, under 1500W power, ultrasonic extraction 1 hour; After ultrasonic end, close stirring, within 60 second time, solution is extracted in upper strata and emit, in leftover materials, add 500Kg edible ethanol, in 40KHz frequency, under 1000W power, ultrasonic extraction 1 hour; After ultrasonic end, close stirring, emit upper strata and extract solution, Bing Jiang lower floor melt cinder is put into squeezer and is carried out Separation of Solid and Liquid, obtains extract and extracts residue 70Kg.
(4) collect the upper strata that step (3) obtains and extract the about 1600Kg of solution, join in low-temperature and high-speed centrifuge, at 10 ℃ of temperature, centrifugation obtains 1. 2. 1570Kg of 30Kg and clear liquid of solid content.
(5) by the clear liquid in step (4) 2. 35 ℃ of temperature, under 10KPa pressure, carry out Vacuum Concentration and reclaim edible ethanol, until be concentrated to 100Kg solution, add in interlayer crystallizing tank, in 0 ℃ of crystallization, except sugar, obtain agate coffee and extract 3. 1.2Kg of concentrate.
(6) 1. 30Kg solid content is joined and stir to extract in still, adding volumn concentration is 75% edible ethanol 150Kg, at 90 ℃ of temperature, stir and extract 1 hour, standing 25 minutes, Separation of Solid and Liquid, repeated to extract twice, merge extract, the extract that obtains 235Kg, joins in vacuum concentrator, 45 ℃ of temperature, 10KPa vacuum under pressure is concentrated, obtains 4. 0.65Kg of concentrate.
(7) the extraction residue in step (3) is poured into and extracted in still, add 350Kg pure water, at 60 ℃ of temperature, the ultrasonic lower extraction of 25kHz step three times, obtains extract 1000Kg, in 45 ℃ of temperature, 10KPa vacuum under pressure is concentrated into 50Kg, the edible ethanol that the volumn concentration that adds again 150Kg is 95%, standing 5 hours, collects and obtains 5. 0.35Kg of precipitation concentrate.
(8) merge agate coffee extract concentrate 3., concentrate 4. with concentrate 5., obtain agate coffee extract 2.2Kg, in this 2.2Kg agate coffee extract, contain agate coffee alkene, agate coffee acid amides, polysaccharide, sterol and the about 310g of glucosinolate.
Embodiment 2.
In the present embodiment, the preparation method of agate coffee extract comprises the steps.
(1) take moisture content and be no more than 5% agate coffee piece undercut sheet 200Kg.
(2) agate coffee sheet is crushed to 400 object fineness, the pueraria root powder crushing is added in the ultrasonic extraction still of interlayer, add 1400Kg edible ethanol, under the mixing speed of 60 revs/min, at 35 ℃ of temperature, 20KHz frequency, under 1600W power, ultrasonic extraction 1.5 hours.
(3) after ultrasonic end, close stirring, within 90 second time, solution is extracted in upper strata and emit, in leftover materials, add 1000Kg edible ethanol, in 20KHz frequency, under 1600W power, ultrasonic extraction 1.5 hours; After ultrasonic end, close stirring, within 90 second time, solution is extracted in upper strata and emit, in leftover materials, add 1000Kg edible ethanol, in 45KHz frequency, under 1000W power, ultrasonic extraction 1 hour; After ultrasonic end, close stirring, emit upper strata and extract solution, Bing Jiang lower floor melt cinder is put into squeezer and is carried out Separation of Solid and Liquid, obtains and extracts solution and extract residue 160Kg.
(4) collect the upper strata that step (3) obtains and extract the about 3200Kg of solution, join in continuous low-temperature supercentrifuge, at 10 ℃ of temperature, centrifugation obtains 1. 2. 3140Kg of 60Kg and clear liquid of solid content.
(5) by clear liquid 2. 35 ℃ of temperature, under 10KPa pressure, carry out Vacuum Concentration and reclaim edible ethanol, until be concentrated to 150Kg solution, add in interlayer crystallizing tank, at 0 ℃ of temperature, crystallization, except sugar, obtains agate coffee and extracts 3. 2.0Kg of concentrate.
(6) 1. 60Kg solid content is joined and stir to extract still, adding volumn concentration is 75% edible ethanol 300Kg, at 90 ℃ of temperature, stir and extract 1 hour, standing 25 minutes, Separation of Solid and Liquid, repeated to extract twice, merge extract, the extract that obtains 580Kg, joins extract in vacuum concentrator, 45 ℃ of temperature, 10KPa vacuum under pressure is concentrated, obtains 4. 1.1Kg of concentrate.
(7) the extraction residue in step (3) is poured into and extracted in still, add 900Kg pure water, at 60 ℃ of temperature, the ultrasonic lower extraction of 25kHz step three times, obtains extract 2700Kg, in 45 ℃ of temperature, 10KPa vacuum under pressure is concentrated into 140Kg, the edible ethanol that the volumn concentration that adds again 400Kg is 95%, standing 5 hours, collects and obtains 5. 0.8Kg of precipitation concentrate.
(8) merge agate coffee extract concentrate 3., concentrate 4. with concentrate 5., obtain agate coffee extract 3.9Kg, in this 3.9Kg agate coffee extract, contain agate coffee alkene, agate coffee acid amides, polysaccharide, sterol and the about 910g of glucosinolate.
Embodiment 3.
The preparation method of the agate coffee extract in the present embodiment comprises the steps.
(1) by agate coffee piece undercut sheet, obtain agate coffee sheet, the moisture content of agate coffee sheet is 2～5%.
(2) agate coffee sheet is pulverized, obtain pueraria root powder, pueraria root powder is added in the ultrasonic extraction still of interlayer, add edible ethanol, the weight ratio of pueraria root powder and edible ethanol is 1:5～1:10 again, and low whipping speed is 60 revs/min, temperature is 5～40 ℃, frequency is 20～45KHz, under the condition that power is 1000～1700W, and ultrasonic extraction 1～2 hour.Generally, agate coffee sheet is crushed to 300～500 object fineness.
(3) after the ultrasonic extraction of step (2) finishes, close stirring, within 30～90 second time, solution being extracted in upper strata emits, in leftover materials, add edible ethanol, the weight of the edible ethanol adding is 3-7 times of pueraria root powder weight, and low whipping speed is 60 revs/min, temperature is 5～40 ℃, frequency is 20～45KHz, under the condition that power is 1000～1700W, and ultrasonic extraction 1～2 hour.
(4) after the ultrasonic extraction of step (3) finishes, close stirring, within 30～90 second time, solution being extracted in upper strata emits, in leftover materials, add edible ethanol, the weight of the edible ethanol adding is 3-7 times of pueraria root powder weight, and low whipping speed is 60 revs/min, temperature is 5～40 ℃, frequency is 20～45KHz, under the condition that power is 1000～1700W, and ultrasonic extraction 1～2 hour.
(5) after the ultrasonic extraction of step (4) finishes, close stirring, pour material in still in solid-liquid separating machine expression separation, obtain upper strata and extract solution and extract residue.
(6) solution is extracted on combining step (3), (4) and (5) obtain upper strata, and solution is extracted in this upper strata joins in low-temperature and high-speed centrifuge, at 5～15 ℃ of temperature, centrifugation obtain solid content 1. with clear liquid 2..
(7) by clear liquid 2. 35 ℃ of temperature, under 10KPa pressure, carry out Vacuum Concentration, reclaim edible ethanol and crystallization except sugar, obtain and extract concentrate 3., 3. this extraction concentrate comprises agate coffee alkene, agate coffee acid amides and sterol.
(8) 1. solid content is joined and stir in extraction still, adding volumn concentration is 75% edible ethanol, 1. solid content is 1:4～1:6 with the weight ratio of the volumn concentration edible ethanol that is 75%, at 90 ℃ of temperature, stir and extract 1 hour, standing 25 minutes, Separation of Solid and Liquid, obtained extract and solid content.Generally, 1. solid content is 1:5 with the weight ratio of the volumn concentration edible ethanol that is 75%.
(9) to adding volumn concentration in the solid content of step (8), be 75% edible ethanol, the weight ratio of the edible ethanol that solid content and volumn concentration are 75% is 1:4～1:6, at 90 ℃ of temperature, stir and extract 1 hour, standing 25 minutes, Separation of Solid and Liquid, obtained extract and solid content.The weight ratio of the edible ethanol that generally, solid content and volumn concentration are 75% is 1:5.
(10) extract that combining step (8) and (9) obtain, 45 ℃ of temperature, 10KPa vacuum under pressure is concentrated, obtains and extracts concentrate 4., and 4. this extraction concentrate comprises glucosinolate.
(11) to the pure water that adds 5 times of volumes in the extraction residue of step (5), at 60 ℃, ultrasonic extraction three times, merge extract, Vacuum Concentration is removed 90% moisture content, then adds the edible ethanol that the volumn concentration of 3 times of volumes is 95%, standing 5 hours, 5. collecting precipitation, to extract concentrate, and this extraction concentrate mainly comprises the thick polysaccharide of agate coffee in 5..
(12) the extraction concentrate of the extraction concentrate of the extraction concentrate in combining step (7) 3., in step (10) 4. and in step (11) 5., obtains agate coffee extract.
Generally, in step (2) and step (3), the power of ultrasonic extraction is 1500W～1700W, and in step (4), the power of ultrasonic extraction is 1000-1200W; In step (2) and step (3), the frequency of ultrasonic extraction is 20-25KHz, and in step (4), the frequency of ultrasonic extraction is 35-45KHz.
The present embodiment also relates to a kind of agate coffee extract being made by above-mentioned preparation method, and this agate coffee extract application on food, health product and medicine.
Embodiment 4.
The preparation method of the agate coffee extract in the present embodiment comprises the steps.
(1) select ripe agate coffee piece root, with drinking water, clean up, section is dried to moisture content 2～5% at 45 ℃ of temperature.This step is by agate coffee raw material drying to the lower state of moisture content, and next step adopts pure edible ethanol to extract, and the too high crystallization that can affect after extracting of moisture content removes sugared efficiency.
(2) dried agate coffee sheet is crushed to 300～500 orders, the pueraria root powder crushing is added in the ultrasonic extraction still of interlayer, the edible ethanol that adds 5-10 times of pueraria root powder weight, under the mixing speed of 60 revs/min, at 5～40 ℃ of temperature, 20～45KHz frequency, under 1000～1700W power, ultrasonic extraction 1～2 hour.This step first will be dried agate coffee sheet and be crushed to 300～500 object fineness, the particle diameter of 20～40 μ m, and in ultrasonic leaching process, the particle of this yardstick, is easy to starch granules in pueraria root powder to separate out.The supersonic frequency of 20～45KHz, the ultrasonic power of 1000～1700W, powerful ultrasonic, can produce stronger cavitation demolition effect, also make starch granules more easily be precipitated, compared with low temperature, guarantee that extract can excessively not heat up because of ultrasonication, make the easier strippings of effective ingredient such as agate coffee alkene and agate coffee acid amides, at lower temperature, extract more thoroughly, so both guaranteed recovery rate, make again the active ingredient can Yin Gaowen and inactivation.The ethanol of 100% purity, as extracting solvent, can extract 1～3 glucosyl group oligosaccharides under the ultrasonic state of low temperature, maca polysaccharide can not extracted again, is conducive to follow-up crystallization except sugared process.
(3) after ultrasonic end, close stirring, within 30～90 second time, solution is extracted in upper strata and emit, to the edible ethanol that adds 3-7 times of pueraria root powder weight in leftover materials, twice of the extraction separation process of repeating step (2) and step (3).Inventor studies discovery, in the ultrasonic leaching process of agate coffee, and the starch granules absorption that effective ingredient glucosinolate compounds is more easily precipitated, and in starch granules, substantially do not contain the compositions such as agate coffee alkene, agate coffee acid amides and polysaccharide.In after ultrasonic end 30～90 seconds of this step, solution being extracted in upper strata emits, starch granules is flowed out together with extract, at next step, carry out separation, undermost solid content is added to edible ethanol again and repeat to extract, be finally added to and in solid-liquid separating machine, carry out melt cinder separation.
(4) collect upper strata and extract solution, and join low-temperature and high-speed centrifuge, at 5～15 ℃ of temperature, centrifugation obtain solid content 1. with clear liquid 2..1. the solid content that this step obtains the upper strata extraction solution centrifugal separation of extraction is mainly starch granules and glucosinolate compounds, and 2. the clear liquid obtaining is mainly agate coffee ethanol extract.
(5) by solution 2. 35 ℃ of temperature, under 10KPa pressure, carry out Vacuum Concentration and reclaim edible ethanol, crystallization except sugar, obtain agate coffee and extract concentrate 3..This step reclaims edible ethanol by agate coffee ethanol extract, and crystallization is except sugar, obtains agate coffee alkene, agate coffee acid amides and sterol and extracts concentrate.
(6) 1. solid content is joined and stir in extraction still, add 5 times of solid contents edible ethanol that 1. volumn concentration of weight is 75%, at 90 ℃ of temperature, stir and extract 1 hour, standing 25 minutes, Separation of Solid and Liquid, repeat to extract twice, merge extract, 45 ℃ of temperature, 10KPa vacuum under pressure is concentrated, obtains concentrate 4..This step water alcohol mixed extract at 90 ℃ of temperature extracts the glucosinolate compounds in starch granules, and Vacuum Concentration obtains glucosinolate extract.
(7) the extraction residue in step (3) is poured into and stirred in extraction still, the pure water that adds 5 times of volumes, at 60 ℃, ultrasonic extraction three times, merges extract, Vacuum Concentration is removed 90% moisture content, the edible ethanol that the volumn concentration that adds again 3 times of volumes is 95%, standing 5 hours, collecting precipitation, obtain concentrate 5., mainly comprise the thick polysaccharide of agate coffee.
(8) merge agate coffee extract concentrate 3., concentrate 4. with concentrate 5., be agate coffee extract.The total amount of the agate coffee alkene that said extracted arrives, agate coffee acid amides, polysaccharide, sterol and glucosinolate surpasses 10% agate coffee extract.
Generally, in step (2) and step (3), extracting for the first time and for the second time ultrasonic power is 1500W～1700W, and the ultrasonic power extracting is for the third time 1000-1200W; Extract for the first time and for the second time, adopt high-power high sound pressure ultrasonic, can produce large cavitation bubble, cavitation intensity is large, the fragmentation that is beneficial to material is extracted, and in adopting for the third time, the low acoustic pressure of power is ultrasonic, can produce little and fine and closely woven cavitation bubble, cavitation intensity is smaller, but is beneficial to the extraction of active principle in small material.The described ultrasonic extraction frequency of step (2) and step (3), for the first time and for the second time supersonic frequency is 20-25KHz, supersonic frequency is 35-45KHz for the third time; For the first time with secondary ultrasonic extraction, adopt low frequency ultrasound, can produce large cavitation bubble, the ratio of bubble full-size and initial size is large, cavitation intensity is large, be conducive to the broken of initial material and extract, ultrasonic extraction for the third time, adopts high frequency ultrasound, produce fine and closely woven cavitation bubble, the ratio of bubble full-size and initial size is little, and number of bubbles is many during than low frequency, is of value to the extraction of active principle in small particles material.
Although the present invention with embodiment openly as above; but it is not in order to limit protection scope of the present invention; any technical staff who is familiar with this technology, not departing from change and the retouching of doing in the spirit and scope of the present invention, all should belong to protection scope of the present invention.
Claims (10)
1. a preparation method for agate coffee extract, is characterized in that: comprise the steps:
(1) by agate coffee piece undercut sheet, obtain agate coffee sheet, the moisture content of agate coffee sheet is 2～5%;
(2) agate coffee sheet is pulverized, obtain pueraria root powder, pueraria root powder is added in the ultrasonic extraction still of interlayer, add edible ethanol, the weight ratio of pueraria root powder and edible ethanol is 1:5～1:10 again, and low whipping speed is 60 revs/min, temperature is 5～40 ℃, frequency is 20～45KHz, under the condition that power is 1000～1700W, and ultrasonic extraction 1～2 hour;
(3) after the ultrasonic extraction of step (2) finishes, close stirring, within 30～90 second time, solution being extracted in upper strata emits, in leftover materials, add edible ethanol, the weight of the edible ethanol adding is 3-7 times of pueraria root powder weight, and low whipping speed is 60 revs/min, temperature is 5～40 ℃, frequency is 20～45KHz, under the condition that power is 1000～1700W, and ultrasonic extraction 1～2 hour;
(4) after the ultrasonic extraction of step (3) finishes, close stirring, within 30～90 second time, solution being extracted in upper strata emits, in leftover materials, add edible ethanol, the weight of the edible ethanol adding is 3-7 times of pueraria root powder weight, and low whipping speed is 60 revs/min, temperature is 5～40 ℃, frequency is 20～45KHz, under the condition that power is 1000～1700W, and ultrasonic extraction 1～2 hour;
(5) after the ultrasonic extraction of step (4) finishes, close stirring, pour material in still in solid-liquid separating machine expression separation, obtain upper strata and extract solution and extract residue;
(6) solution is extracted on combining step (3), (4) and (5) obtain upper strata, and solution is extracted in the upper strata of this merging joins in low-temperature and high-speed centrifuge, at 5～15 ℃ of temperature, centrifugation obtain solid content 1. with clear liquid 2.;
(7) by clear liquid 2. 35 ℃ of temperature, under 10KPa pressure, carry out Vacuum Concentration, reclaim edible ethanol and crystallization except sugar, obtain and extract concentrate 3., 3. this extraction concentrate comprises agate coffee alkene, agate coffee acid amides and sterol;
(8) 1. solid content is joined and stir in extraction still, adding volumn concentration is 75% edible ethanol, 1. solid content is 1:4～1:6 with the weight ratio of the volumn concentration edible ethanol that is 75%, at 90 ℃ of temperature, stir and extract 1 hour, standing 25 minutes, Separation of Solid and Liquid, obtained extract and solid content;
(9) to adding volumn concentration in the solid content of step (8), be 75% edible ethanol, the weight ratio of the edible ethanol that solid content and volumn concentration are 75% is 1:4～1:6, at 90 ℃ of temperature, stir and extract 1 hour, standing 25 minutes, Separation of Solid and Liquid, obtained extract and solid content;
(10) extract that combining step (8) and (9) obtain, 45 ℃ of temperature, 10KPa vacuum under pressure is concentrated, obtains and extracts concentrate 4., and 4. this extraction concentrate comprises glucosinolate;
(11) to the pure water that adds 5 times of volumes in the extraction residue of step (5), at 60 ℃, ultrasonic extraction three times, merge extract, Vacuum Concentration is removed 90% moisture content, then adds the edible ethanol that the volumn concentration of 3 times of volumes is 95%, standing 5 hours, 5. collecting precipitation, to extract concentrate, and this extraction concentrate mainly comprises the thick polysaccharide of agate coffee in 5.;
(12) the extraction concentrate of the extraction concentrate of the extraction concentrate in combining step (7) 3., in step (10) 4. and in step (11) 5., obtains agate coffee extract.
2. the preparation method of agate coffee extract according to claim 1, is characterized in that: in step (2), agate coffee sheet is crushed to 300～500 object fineness.
3. the preparation method of agate coffee extract according to claim 1, is characterized in that: in step (2) and step (3), the power of ultrasonic extraction is 1500W～1700W, and in step (4), the power of ultrasonic extraction is 1000-1200W.
4. the preparation method of agate coffee extract according to claim 1, is characterized in that: in step (2) and step (3), the frequency of ultrasonic extraction is 20-25KHz, and in step (4), the frequency of ultrasonic extraction is 35-45KHz.
5. the preparation method of agate coffee extract according to claim 1, is characterized in that: in step (8), 1. solid content is 1:5 with the weight ratio of the volumn concentration edible ethanol that is 75%.
6. the preparation method of agate coffee extract according to claim 1, is characterized in that: in step (9), the weight ratio of the edible ethanol that solid content and volumn concentration are 75% is 1:5.
7. an agate coffee extract, is characterized in that: adopt the preparation method as described in claim as arbitrary in claim 1-6 to make.
8. the application of agate coffee extract described in claim 7, is characterized in that: this agate coffee extract application on food.
9. the application of agate coffee extract described in claim 7, is characterized in that: this agate coffee extract application on health product.
10. the application of agate coffee extract described in claim 7, is characterized in that: this agate coffee extract application on medicine.
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