CN109010615A - The preparation method of cold soluble type dendrobium candidum extract - Google Patents
The preparation method of cold soluble type dendrobium candidum extract Download PDFInfo
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- CN109010615A CN109010615A CN201810958578.6A CN201810958578A CN109010615A CN 109010615 A CN109010615 A CN 109010615A CN 201810958578 A CN201810958578 A CN 201810958578A CN 109010615 A CN109010615 A CN 109010615A
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- dendrobium candidum
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- 241000026010 Dendrobium candidum Species 0.000 title claims abstract description 91
- 239000000284 extract Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 163
- 239000007788 liquid Substances 0.000 claims description 79
- 235000019441 ethanol Nutrition 0.000 claims description 72
- 239000011347 resin Substances 0.000 claims description 50
- 229920005989 resin Polymers 0.000 claims description 50
- 238000010828 elution Methods 0.000 claims description 45
- 230000002745 absorbent Effects 0.000 claims description 35
- 239000002250 absorbent Substances 0.000 claims description 35
- 239000003480 eluent Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 23
- 239000012141 concentrate Substances 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 13
- 239000012530 fluid Substances 0.000 claims description 11
- 108010059892 Cellulase Proteins 0.000 claims description 10
- 229940106157 cellulase Drugs 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000000108 ultra-filtration Methods 0.000 claims description 5
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 5
- 230000015556 catabolic process Effects 0.000 claims description 4
- 238000006731 degradation reaction Methods 0.000 claims description 4
- 108010059820 Polygalacturonase Proteins 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 230000007071 enzymatic hydrolysis Effects 0.000 claims description 3
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- 108010093305 exopolygalacturonase Proteins 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 1
- 150000004676 glycans Chemical class 0.000 abstract description 14
- 229920001282 polysaccharide Polymers 0.000 abstract description 14
- 239000005017 polysaccharide Substances 0.000 abstract description 14
- 241001076416 Dendrobium tosaense Species 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000000857 drug effect Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000007654 immersion Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 7
- 230000009102 absorption Effects 0.000 description 6
- 108090000790 Enzymes Proteins 0.000 description 4
- 102000004190 Enzymes Human genes 0.000 description 4
- 229940088598 enzyme Drugs 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 3
- 241001523681 Dendrobium Species 0.000 description 2
- 240000004638 Dendrobium nobile Species 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 208000002177 Cataract Diseases 0.000 description 1
- 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 1
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 210000002683 foot Anatomy 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 201000001881 impotence Diseases 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 210000003296 saliva Anatomy 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
Classifications
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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)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/898—Orchidaceae (Orchid family)
- A61K36/8984—Dendrobium
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- 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
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The present invention relates to a kind of preparation methods of cold soluble type dendrobium candidum extract, it is the following steps are included: (1) dendrobium candidum crushes immersion；(2) it digests；(3) it filters；(4) it purifies；(5) it is concentrated；(6) cold filtration；(7) powder is dried out up to the cold soluble type dendrobium candidum extract；The present invention has the advantages that preparation method of the invention can obtain the dendrobium candidum extract of good water solubility, this dendrobium candidum extract is a kind of Dendrobium officinale polysaccharide.The dendrobium candidum extract is just rapidly dissolvable in cold water and its minimum solution temperature is up to 8 DEG C, can dissolve the 6g dendrobium candidum extract in 8 DEG C of water of 100g, it can thus be appreciated that dendrobium candidum extract produced by the present invention is a kind of cold soluble type substance.Also just because of the good aqueous solubility of the dendrobium candidum extract, so that it can be used in time research of Dendrobium officinale polysaccharide pharmacology, the deeper of drug effect.
Description
Technical field
The present invention relates to a kind of preparation methods of cold soluble type dendrobium candidum extract.
Background technique
Dendrobium candidum is the perennial type herbaceous plant that grows nonparasitically upon another plant of orchid family Dendrobium, is top grade in dendrobium nobile medicinal material, with sweet in flavor, matter
Heavy, the big person of flexible and stickiness is preferred, and has the effect of reinforcing stomach reg fluid, nourishing Yin and clearing heat, is clinically used for treatment pyreticosis saliva wound, stomach-Yin not
The diseases such as foot, muscles and bones impotence.Modern pharmacology research shows that dendrobium candidum has enhancing to make non-specific and specific immunity
With, it is antitumor, anti-oxidant, reduce blood glucose and cataract in terms of, pharmacological action is significant.The drug effect of dendrobium candidum
Effect is primarily due to it and contains a variety of active ingredients, such as alkaloid, polysaccharide, amino acid, but the effect of various active constituents
But it is not quite similar.And dendrobium candidum clinically mainly worked by taking dendrobium candidum medicinal material tanning decoction of medicinal ingredients by application, respectively
The effect of active constituent, is not applied targetedly, so some researchers carry out the different activities ingredient of dendrobium candidum
Separation is extracted, is dedicated to further developing the medical value of dendrobium candidum.Currently, there are many researcher to Dendrobium officinale polysaccharide into
Row extracts, although there are many Dendrobium officinale polysaccharide that technology has been able to obtain high extraction, these polysaccharide extracted
Water solubility it is bad, affect Dendrobium officinale polysaccharide use and Dendrobium officinale polysaccharide pharmacology, drug efficacy study.
Summary of the invention
The purpose of the present invention is to provide a kind of high extraction and the preparation of cold soluble type dendrobium candidum extract can be obtained
Method.
The purpose of the present invention is achieved through the following technical solutions: a kind of preparation method of cold soluble type dendrobium candidum extract,
It the following steps are included:
(1) dendrobium candidum, which crushes, impregnates: hot-water soak being added after dendrobium candidum is crushed, obtains just feed liquid；
(2) it digests: cellulase degradation is added in the first feed liquid described in step (1), adds pectinase enzymatic hydrolysis later,
Obtain time feed liquid；
(3) it filters: the resulting secondary feed liquid of step (2) being filtered, coarse fodder liquid is obtained；
(4) it purifies: the resulting coarse fodder liquid of step (3) being adsorbed using macroporous absorbent resin, is made later with water-ethanol
It is eluted for eluent, collects efflux；
(5) it is concentrated: the efflux that step (4) are collected being concentrated, concentrate is obtained；
(6) cold filtration: step (5) resulting concentrate being cooled down, is filtered later, is collected filtrate, is obtained whole feed liquid；
(7) it dries out powder: crushing is dried to get the cold soluble type dendrobium candidum in the resulting whole feed liquid of step (6)
Extract.
For the prior art, the present invention has the advantages that preparation method of the invention can obtain good water solubility
Dendrobium candidum extract, this dendrobium candidum extract are a kind of Dendrobium officinale polysaccharides.The dendrobium candidum extract is in cold water
Just rapidly dissolvable and its minimum solution temperature can dissolve the 6g dendrobium candidum extract up to 8 DEG C in 8 DEG C of water of 100g,
At i.e. 8 DEG C, the solubility of the dendrobium candidum extract is 6g/100g water, it can thus be appreciated that dendrobium candidum produced by the present invention extracts
Object is a kind of cold soluble type substance.Also just because of the good aqueous solubility of the dendrobium candidum extract, so that it can be used for dendrobium candidum
In time research of polysaccharide pharmacology, the deeper of drug effect.It can also apply in the processing and fabricating of some health care products or other food,
This polysaccharide soluble type is convenient for absorption of human body.In addition, preparation method of the invention is simple, recovery rate is high.
Specific embodiment
The content of present invention is described in detail below with reference to embodiment:
A kind of preparation method of cold soluble type dendrobium candidum extract, it the following steps are included:
(1) dendrobium candidum, which crushes, impregnates: hot-water soak being added after dendrobium candidum is crushed, obtains just feed liquid；
(2) it digests: cellulase degradation is added in the first feed liquid described in step (1), adds pectinase enzymatic hydrolysis later,
Obtain time feed liquid；
(3) it filters: the resulting secondary feed liquid of step (2) being filtered, coarse fodder liquid is obtained；
(4) it purifies: the resulting coarse fodder liquid of step (3) being adsorbed using macroporous absorbent resin, is made later with water-ethanol
It is eluted for eluent, collects efflux；
(5) it is concentrated: the efflux that step (4) are collected being concentrated, concentrate is obtained；
(6) cold filtration: step (5) resulting concentrate being cooled down, is filtered later, is collected filtrate, is obtained whole feed liquid；
(7) it dries out powder: crushing is dried to get the cold soluble type dendrobium candidum in the resulting whole feed liquid of step (6)
Extract.
Wherein, the concrete operation method of step (1) are as follows:
Dendrobium candidum herb is first crushed to 10~15 mesh, smashed dendrobium candidum is added to 60~80 DEG C of heat later
30~60min is impregnated in water, obtains just feed liquid；Wherein, the solid-liquid ratio of dendrobium candidum and hot water is 1:10~1:15g/mL；
The concrete operation method of step (2) are as follows: the resulting just feed liquid of step (1) is cooled to 40~45 DEG C, is added later
0.05~0.1% cellulase of dendrobium candidum weight is accounted for, 45~60min is reacted；After reaction, it is added and accounts for dendrobium candidum
0.05~0.1% pectase of weight digests 60~90min at 40~45 DEG C, obtains time feed liquid.It is first sharp in step (2)
The cell wall wall of dendrobium candidum cell is abolished with cellulase degradation, the pectin after recycling pectase and broken wall later acts on,
Such enzyme solution can greatly improve enzymolysis efficiency, while improve the recovery rate of dendrobium candidum extract.
The concrete operation method of step (3) are as follows: the resulting secondary feed liquid of step (2) is without cooling, directly first with 40~80
Purpose strainer carries out heat filtering, collects filtered fluid；Filtered fluid recycles 0.2~0.5 μm of ultrafiltration membrane essence filtering later, obtains coarse fodder
Liquid.In step (3), heat filtering is carried out first with the strainer of 40~80 mesh, material residue is removed in separation；Utilize 0.2~0.5 μm surpass
The filtering of filter membrane essence removes remaining processing aid enzyme (remaining cellulase and pectase), is substituted using this method traditional
High temperature enzyme deactivation technique, the effect of can effectively retaining dendrobium candidum ingredient, while enabling dendrobium candidum extract obtained most
The feature flavour of the reservation dendrobium candidum itself of big degree, so that having using food made from the extract in good taste
Advantage.
The concrete operation method of step (4) are as follows: add the resulting coarse fodder liquid of step (3) with the flow velocity of 0.50~1.2BV/h
Enter to filled with macroporous absorbent resin pillar in adsorbed, after the completion of absorption, then successively with water, 10%~20% ethyl alcohol,
30%~50% ethyl alcohol, 60%~90% ethyl alcohol, ethyl alcohol are eluent, carry out gradient elution, entire elution process coutroi velocity
For 0.50~1.2BV/h, eluting temperature is 25~35 DEG C, collects stream when being eluted using 30%~50% ethyl alcohol as eluent
Liquid out；
When being eluted using water as eluent, water elution volume is 2~4 times of macroporous absorbent resin volumes；With 10%~
When 20% ethyl alcohol is that eluent is eluted, 10%~20% ethanol elution volume is 1~3 times of macroporous absorbent resin volume；With
When 30%~50% ethyl alcohol is that eluent is eluted, 30%~50% ethanol elution volume is 5~8 times of macroporous absorbent resin bodies
Product；When being eluted using 60%~90% ethyl alcohol as eluent, 60%~90% ethanol elution volume is 2~3 times of macroporous absorptions
Resin volume；When being eluted using ethyl alcohol as eluent, ethanol elution volume is 1~3 times of macroporous absorbent resin volume；
The macroporous absorbent resin is AB-8 type resin, in D101 type resin, DA-201 type resin, DM-03 type resin
It is a kind of.
Step (4) can obtain the dendrobium candidum of purity is high, good water solubility by the way of gradient elution to the greatest extent
Extract.In addition, the elution fraction of 30%~50% ethyl alcohol has good water solubility, and washed using 30%~50% ethyl alcohol
It is de-, the high dendrobium polysaccharide of number molecular weight can be parsed from macroporous absorbent resin, and the dendrobium nobile that these molecular weight are high
Substance both with precisely a kind of good water solubility of polysaccharide, effect are good.
The concrete operation method of step (5) are as follows: the efflux that step (4) are collected is concentrated in vacuo and is recycled ethyl alcohol,
The concentration that concentrate and concentrate are obtained after concentration is 15~30Brix.
The concrete operation method of step (6) are as follows: step (5) resulting concentrate is cooled to 2~8 DEG C and at this temperature
20~26h is stood, is filtered to remove the object of precipitation later, filtrate is collected, obtains whole feed liquid.
Step (6) removes some low temperature indissoluble polysaccharide by the way of low temperature recrystallization, and resulting dendrobium candidum is allowed to extract
Object also has higher solubility in low temperature.
The concrete operation method of step (7) are as follows: the resulting whole feed liquid of step (6) is first placed in -10~-20 DEG C of freezer unit
Middle 5~8h of pre-freeze, 5~12h of vacuum freeze drying at being then -30 DEG C~-40 DEG C in temperature, distillation 12~for 24 hours, obtain dried object
Material, later crushes dried material, smashed powder crosses the vibration screen of 30~60 mesh to get the cold soluble type iron sheet
Herba Dendrobii extract.
Finer description is made to the contents of the present invention combined with specific embodiments below:
Embodiment one:
A kind of preparation method of cold soluble type dendrobium candidum extract, it the following steps are included:
(1) dendrobium candidum, which crushes, impregnates: dendrobium candidum herb being first crushed to 10 mesh, later by smashed dendrobium candidum
It is added in 60 DEG C of hot water and impregnates 30min, obtain just feed liquid；Wherein, the solid-liquid ratio of dendrobium candidum and hot water is 1:10g/mL.
(2) it digests: the resulting just feed liquid of step (1) being cooled to 40 DEG C, is added accounts for dendrobium candidum weight later
0.05% cellulase reacts 45min；After reaction, 0.05% pectase for accounting for dendrobium candidum weight is added, 40
60min is digested at DEG C, obtains time feed liquid.
(3) filter: the resulting secondary feed liquid of step (2) directly carries out heat filtering first with the strainer of 40 mesh without cooling, receives
Collect filtered fluid；Filtered fluid recycles 0.2 μm of ultrafiltration membrane essence filtering later, obtains coarse fodder liquid.
(4) it purifies: the resulting coarse fodder liquid of step (3) is added to the flow velocity of 0.50BV/h filled with macroporous absorbent resin
Pillar in adsorbed, after the completion of absorption, then successively with water, 10% ethyl alcohol, 30% ethyl alcohol, 60% ethyl alcohol, ethyl alcohol be elution
Liquid carries out gradient elution, and entire elution process coutroi velocity is 0.50BV/h, and eluting temperature is 25 DEG C, collects with 30% ethyl alcohol
Efflux when being eluted for eluent；Wherein, when being eluted using water as eluent, water elution volume is that 2 times of macropores are inhaled
Attached resin volume；When being eluted using 10% ethyl alcohol as eluent, 10% ethanol elution volume is 2 times of macroporous absorbent resin bodies
Product；When being eluted using 30% ethyl alcohol as eluent, 30% ethanol elution volume is 5 times of macroporous absorbent resin volumes；With 60%
When ethyl alcohol is that eluent is eluted, 60% ethanol elution volume is 2 times of macroporous absorbent resin volumes；Using ethyl alcohol as eluent into
When row elution, ethanol elution volume is 2 times of macroporous absorbent resin volumes；The macroporous absorbent resin is AB-8 type resin.
(5) be concentrated: by step (4) collect efflux be concentrated in vacuo and recycled ethyl alcohol, after concentration concentrate and
The concentration of concentrate is 15Brix.
(6) cold filtration: step (5) resulting concentrate is cooled to 2 DEG C and stands 20h at this temperature, later mistake
The object being precipitated is filtered out, filtrate is collected, obtains whole feed liquid.
(7) it dries out powder: the resulting whole feed liquid of step (6) being first placed in pre-freeze 5h in -10 DEG C of freezer unit, then in temperature
Degree is vacuum freeze drying 5h at -30 DEG C, and distil 12h, obtains dried material, later crushes dried material, smashed
Powder crosses the vibration screen of 30 mesh to get the cold soluble type dendrobium candidum extract.
Embodiment two:
A kind of preparation method of cold soluble type dendrobium candidum extract, it the following steps are included:
(1) dendrobium candidum, which crushes, impregnates: dendrobium candidum herb being first crushed to 15 mesh, later by smashed dendrobium candidum
It is added in 80 DEG C of hot water and impregnates 60min, obtain just feed liquid；Wherein, the solid-liquid ratio of dendrobium candidum and hot water is 1:15g/mL.
(2) it digests: the resulting just feed liquid of step (1) being cooled to 45 DEG C, is added accounts for the 0.1% of dendrobium candidum weight later
Cellulase, react 60min；After reaction, 0.1% pectase for accounting for dendrobium candidum weight, the enzyme at 45 DEG C is added
90min is solved, time feed liquid is obtained.
(3) filter: the resulting secondary feed liquid of step (2) directly carries out heat filtering first with the strainer of 80 mesh without cooling, receives
Collect filtered fluid；Filtered fluid recycles 0.5 μm of ultrafiltration membrane essence filtering later, obtains coarse fodder liquid.
(4) it purifies: the resulting coarse fodder liquid of step (3) is added to the flow velocity of 1.2BV/h filled with macroporous absorbent resin
Pillar in adsorbed, after the completion of absorption, then successively with water, 20% ethyl alcohol, 50% ethyl alcohol, 90% ethyl alcohol, ethyl alcohol be elution
Liquid carries out gradient elution, and entire elution process coutroi velocity is 1.2BV/h, and eluting temperature is 35 DEG C, and collection is with 50% ethyl alcohol
Efflux when eluent is eluted.
When being eluted using water as eluent, water elution volume is 4 times of macroporous absorbent resin volumes；It is to wash with 20% ethyl alcohol
When de- liquid is eluted, 20% ethanol elution volume is 3 times of macroporous absorbent resin volumes；It is washed using 50% ethyl alcohol as eluent
When de-, 50% ethanol elution volume is 8 times of macroporous absorbent resin volumes；When being eluted using 90% ethyl alcohol as eluent, 90%
Ethanol elution volume is 3 times of macroporous absorbent resin volumes；When being eluted using ethyl alcohol as eluent, ethanol elution volume is 3 times
Macroporous absorbent resin volume；The macroporous absorbent resin is DA-201 type resin.
(5) be concentrated: by step (4) collect efflux be concentrated in vacuo and recycled ethyl alcohol, after concentration concentrate and
The concentration of concentrate is 30Brix.
(6) cold filtration: step (5) resulting concentrate is cooled to 8 DEG C and stands 26h at this temperature, later mistake
The object being precipitated is filtered out, filtrate is collected, obtains whole feed liquid.
(7) it dries out powder: the resulting whole feed liquid of step (6) being first placed in pre-freeze 8h in -20 DEG C of freezer unit, then in temperature
Degree is vacuum freeze drying 12h at -40 DEG C, and distillation for 24 hours, obtains dried material, later crushes dried material, smashed
Powder crosses the vibration screen of 60 mesh to get the cold soluble type dendrobium candidum extract.
Embodiment three:
A kind of preparation method of cold soluble type dendrobium candidum extract, it the following steps are included:
(1) dendrobium candidum, which crushes, impregnates: dendrobium candidum herb being first crushed to 12 mesh, later by smashed dendrobium candidum
It is added in 70 DEG C of hot water and impregnates 45min, obtain just feed liquid；Wherein, the solid-liquid ratio of dendrobium candidum and hot water is 1:12g/mL.
(2) it digests: the resulting just feed liquid of step (1) being cooled to 43 DEG C, is added accounts for dendrobium candidum weight later
0.08% cellulase reacts 50min；After reaction, 0.08% pectase for accounting for dendrobium candidum weight is added, 43
80min is digested at DEG C, obtains time feed liquid.
(3) filter: the resulting secondary feed liquid of step (2) directly carries out heat filtering first with the strainer of 50 mesh without cooling, receives
Collect filtered fluid；Filtered fluid recycles 0.3 μm of ultrafiltration membrane essence filtering later, obtains coarse fodder liquid.
(4) it purifies: the resulting coarse fodder liquid of step (3) is added to the flow velocity of 1.0BV/h filled with macroporous absorbent resin
Pillar in adsorbed, after the completion of absorption, then successively with water, 15% ethyl alcohol, 45% ethyl alcohol, 75% ethyl alcohol, ethyl alcohol be elution
Liquid carries out gradient elution, and entire elution process coutroi velocity is 1.0BV/h, and eluting temperature is 30 DEG C, and collection is with 45% ethyl alcohol
Efflux when eluent is eluted；
Wherein, when being eluted using water as eluent, water elution volume is 3 times of macroporous absorbent resin volumes；With 15% second
When alcohol is that eluent is eluted, 15% ethanol elution volume is 2 times of macroporous absorbent resin volumes；Using 45% ethyl alcohol as eluent
When being eluted, 45% ethanol elution volume is 6 times of macroporous absorbent resin volumes；It is eluted using 75% ethyl alcohol as eluent
When, 75% ethanol elution volume is 2 times of macroporous absorbent resin volumes；When being eluted using ethyl alcohol as eluent, ethanol elution body
Product is 2 times of macroporous absorbent resin volumes；The macroporous absorbent resin is D101 type resin.
(5) be concentrated: by step (4) collect efflux be concentrated in vacuo and recycled ethyl alcohol, after concentration concentrate and
The concentration of concentrate is 20Brix.
(6) cold filtration: step (5) resulting concentrate is cooled to 5 DEG C and is stood at this temperature for 24 hours, later mistake
The object being precipitated is filtered out, filtrate is collected, obtains whole feed liquid.
(7) it dries out powder: the resulting whole feed liquid of step (6) being first placed in pre-freeze 6h in -15 DEG C of freezer unit, then in temperature
Degree is vacuum freeze drying 10h at -35 DEG C, and distil 15h, obtains dried material, later crushes dried material, smashed
Powder crosses the vibration screen of 50 mesh to get the cold soluble type dendrobium candidum extract.
It should be noted that above embodiments are only used for illustrating the contents of the present invention, and it is not intended to the limitation present invention
Protection scope.Furthermore, it is to be understood that after reading the technical contents of the present invention, those skilled in the art can be to this hair
Bright to make various change, modification and/or variation, all these equivalent forms equally fall within the application the appended claims and are limited
Within fixed protection scope.
Claims (10)
1. a kind of preparation method of cold soluble type dendrobium candidum extract, it is characterised in that: it the following steps are included:
(1) dendrobium candidum, which crushes, impregnates: hot-water soak being added after dendrobium candidum is crushed, obtains just feed liquid；
(2) it digests: cellulase degradation is added in the first feed liquid described in step (1), adds pectinase enzymatic hydrolysis later, obtain secondary
Feed liquid；
(3) it filters: the resulting secondary feed liquid of step (2) being filtered, coarse fodder liquid is obtained；
(4) it purifies: the resulting coarse fodder liquid of step (3) is adsorbed using macroporous absorbent resin, later using water-ethanol as washing
De- liquid is eluted, and efflux is collected；
(5) it is concentrated: the efflux that step (4) are collected being concentrated, concentrate is obtained；
(6) cold filtration: step (5) resulting concentrate being cooled down, is filtered later, is collected filtrate, is obtained whole feed liquid；
(7) it dries out powder: crushing is dried to get cold soluble type dendrobium candidum extraction in the resulting whole feed liquid of step (6)
Object.
2. the preparation method of cold soluble type dendrobium candidum extract according to claim 1, it is characterised in that: step (1)
Concrete operation method are as follows:
Dendrobium candidum herb is first crushed to 10~15 mesh, smashed dendrobium candidum is added later in 60~80 DEG C of hot water
30~60min is impregnated, just feed liquid is obtained；Wherein, the solid-liquid ratio of dendrobium candidum and hot water is 1:10~1:15g/mL.
3. the preparation method of cold soluble type dendrobium candidum extract according to claim 1, it is characterised in that: step (2)
Concrete operation method are as follows: the resulting just feed liquid of step (1) is cooled to 40~45 DEG C, is added accounts for dendrobium candidum weight later
0.05~0.1% cellulase reacts 45~60min；After reaction, be added account for dendrobium candidum weight 0.05~
0.1% pectase digests 60~90min at 40~45 DEG C, obtains time feed liquid.
4. the preparation method of cold soluble type dendrobium candidum extract according to claim 1, it is characterised in that: step (3)
Concrete operation method are as follows: the resulting secondary feed liquid of step (2) directly carries out hot mistake first with the strainer of 40~80 mesh without cooling
Filtered fluid is collected in filter；Filtered fluid recycles 0.2~0.5 μm of ultrafiltration membrane essence filtering later, obtains coarse fodder liquid.
5. the preparation method of cold soluble type dendrobium candidum extract according to claim 1, it is characterised in that: step (4)
Concrete operation method are as follows: be added to the resulting coarse fodder liquid of step (3) filled with macroporous absorption with the flow velocity of 0.50~1.2BV/h
It is adsorbed in the pillar of resin, after the completion of absorption, then successively with water, 10%~20% ethyl alcohol, 30%~50% ethyl alcohol, 60%
~90% ethyl alcohol, ethyl alcohol are eluent, carry out gradient elution, and entire elution process coutroi velocity is 0.50~1.2BV/h, elution
Temperature is 25~35 DEG C, collects efflux when being eluted using 30%~50% ethyl alcohol as eluent.
6. the preparation method of cold soluble type dendrobium candidum extract according to claim 5, it is characterised in that: with water be elution
When liquid is eluted, water elution volume is 2~4 times of macroporous absorbent resin volumes；It is carried out by eluent of 10%~20% ethyl alcohol
When elution, 10%~20% ethanol elution volume is 1~3 times of macroporous absorbent resin volume；It is elution with 30%~50% ethyl alcohol
When liquid is eluted, 30%~50% ethanol elution volume is 5~8 times of macroporous absorbent resin volumes；With 60%~90% ethyl alcohol
When being eluted for eluent, 60%~90% ethanol elution volume is 2~3 times of macroporous absorbent resin volumes；It is to wash with ethyl alcohol
When de- liquid is eluted, ethanol elution volume is 1~3 times of macroporous absorbent resin volume.
7. the preparation method of cold soluble type dendrobium candidum extract according to claim 5, it is characterised in that: the macropore is inhaled
Attached resin is one of AB-8 type resin, D101 type resin, DA-201 type resin, DM-03 type resin.
8. the preparation method of cold soluble type dendrobium candidum extract according to claim 1, it is characterised in that: step (5)
Concrete operation method are as follows: the efflux that step (4) are collected is concentrated in vacuo and is recycled ethyl alcohol, after concentration concentrate and dense
The concentration of contracting liquid is 15~30Brix.
9. the preparation method of cold soluble type dendrobium candidum extract according to claim 1, it is characterised in that: step (6)
Concrete operation method are as follows: step (5) resulting concentrate is cooled to 2~8 DEG C and stands 20~26h at this temperature, later
It is filtered to remove the object of precipitation, filtrate is collected, obtains whole feed liquid.
10. the preparation method of cold soluble type dendrobium candidum extract according to claim 1, it is characterised in that: step (7)
Concrete operation method are as follows: the resulting whole feed liquid of step (6) is first placed in 5~8h of pre-freeze in -10~-20 DEG C of freezer unit, then
5~12h of vacuum freeze drying at being -30 DEG C~-40 DEG C in temperature, distillation 12~for 24 hours, dried material is obtained, later by dried object
Material is crushed, and smashed powder crosses the vibration screen of 30~60 mesh to get the cold soluble type dendrobium candidum extract.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109620787A (en) * | 2019-01-30 | 2019-04-16 | 广州诗美化妆品有限公司 | A kind of moisturizing golden hairpin dendrobium extract and the preparation method and application thereof |
| CN109793692A (en) * | 2019-02-27 | 2019-05-24 | 苏州天成新农生物科技有限公司 | Filter method suitable for the dry bud stoste of dendrobium candidum |
| CN109793691A (en) * | 2019-02-27 | 2019-05-24 | 苏州天成新农生物科技有限公司 | Filter method suitable for dendrobium candidum tender shoots stoste |
| CN112409500A (en) * | 2019-08-23 | 2021-02-26 | 衢州市展宏生物科技有限公司 | Dendrobium officinale water-soluble polysaccharide powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109620787A (en) * | 2019-01-30 | 2019-04-16 | 广州诗美化妆品有限公司 | A kind of moisturizing golden hairpin dendrobium extract and the preparation method and application thereof |
| CN109793692A (en) * | 2019-02-27 | 2019-05-24 | 苏州天成新农生物科技有限公司 | Filter method suitable for the dry bud stoste of dendrobium candidum |
| CN109793691A (en) * | 2019-02-27 | 2019-05-24 | 苏州天成新农生物科技有限公司 | Filter method suitable for dendrobium candidum tender shoots stoste |
| CN112409500A (en) * | 2019-08-23 | 2021-02-26 | 衢州市展宏生物科技有限公司 | Dendrobium officinale water-soluble polysaccharide powder |
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