CN109336738A - A kind of preparation method of arabite - Google Patents

A kind of preparation method of arabite Download PDF

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Publication number
CN109336738A
CN109336738A CN201811361361.3A CN201811361361A CN109336738A CN 109336738 A CN109336738 A CN 109336738A CN 201811361361 A CN201811361361 A CN 201811361361A CN 109336738 A CN109336738 A CN 109336738A
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China
Prior art keywords
molecular weight
reverse osmosis
arabite
alcohol
dehydrated alcohol
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CN201811361361.3A
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Chinese (zh)
Inventor
周帅
唐庆九
张劲松
冯娜
张忠
杨焱
刘艳芳
贾薇
唐传红
刘方
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Shanghai Academy of Agricultural Sciences
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Shanghai Academy of Agricultural Sciences
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Priority to CN201811361361.3A priority Critical patent/CN109336738A/en
Publication of CN109336738A publication Critical patent/CN109336738A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/78Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The invention discloses a kind of preparation methods of arabite, and this method comprises the following steps: the nanofiltration that edible fungi extract carries out 500 molecular weight is operated;Collect the part less than 500 molecular weight;Extracting solution less than 500 molecular weight is subjected to reverse osmosis membrane filtration operation;Feed liquid is concentrated into its soluble solid content and reaches 40-50%, dehydrated alcohol is added and is crystallized, filters, obtains coarse crystallization;It is heated to dissolving after coarse crystallization is mixed with dehydrated alcohol by 1:20 weight ratio, stand, naturally cool to recrystallization, drying after suction filtration obtains the sugar alcohol crystal of high-purity.The preparation method of arabite of the invention is easy to operate, the arabite purity is high being prepared.

Description

A kind of preparation method of arabite
Technical field
The present invention relates to Edible mushroom processing fields, more particularly to a kind of preparation method of arabite.
Background technique
For edible mushroom as a kind of macro fungi, carbohydrate content therein is very high, typically constitutes from 60% of dry weight or so, Wherein sugar alcohol substance such as arabite (Arabinitol) is widely present in edible mushroom, in needle mushroom, Hericium erinaceus Content in fructification is up to 10%, and the content in ganoderma lucidum fruitbody is up to 5%.Sugar alcohol (Sugar alcohol) is also referred to as more First alcohol (Polyol) is food, chemical industry and important source material substance pharmaceutically.It can be dissolved in water and hot alcohol, its main feature is that Sugariness is low, heat is low, viscosity is low, and hygroscopicity is larger.Since its metabolic pathway is unrelated with insulin, human body, which takes the photograph people, will not cause blood Sugar and insulin level fluctuation, therefore be the ideal sweetener of diabetes patient;In addition long-term intake will not cause saprodontia, can be used as Chewing gum sweet taste filler;Part sugar alcohol has the function of dietary fiber, can prevent constipation, colon cancer etc..Arabite is still The intermediate of xylose alcohol production can be applied to the production of sweetener.
In the extraction process of edible mushroom, the polysaccharide in macromolecule, the terpene with greater activity, steroid small molecule object After matter is separated, prepared, sugar alcohol substance is still largely present in remaining extracting solution, will form if as do not purified Biggish waste.The preparation method of sugar alcohol constituents mainly has at present: one, chemistry or enzyme process: being obtained using starch or plant cell Corresponding carbohydrate is taken, is obtained by way of reduction.Two, fermentation method: by after the microbial fermentations xylose such as yeast from fermentation liquid In isolate and purify to obtain, since used raw material and xylose are plant origins, what these two kinds of methods obtained be L-type I Primary sugar alcohol, and contained in edible mushroom it is D type arabite, it is less compared with L-type arabite source, it is not easy largely to be obtained ?.
It there is no at present and be related to the arabite prepare with scale technology in edible mushroom source.
Summary of the invention
The invention discloses a kind of preparation methods of arabite, and this method comprises the following steps:
1. 500 molecular weight nanofiltrations;
Edible fungi extract is carried out to the nanofiltration operation of 500 molecular weight;Collect the part less than 500 molecular weight;
2. reverse osmosis membrane filtration
Extracting solution less than 500 molecular weight is subjected to reverse osmosis membrane filtration operation;
3. crystallizing
Feed liquid is concentrated into its soluble solid content to reach 40-50% (weight ratio), dehydrated alcohol is added and is tied Crystalline substance filters, obtains coarse crystallization;
4. recrystallizing
It is heated to dissolving after coarse crystallization is mixed with dehydrated alcohol by 1:20 weight ratio, stands, naturally cool to and tie again Crystalline substance, it is dry after suction filtration, obtain the sugar alcohol crystal of high-purity.
Wherein, the edible fungi extract is that edible mushroom carries out alcohol extracting (85% ethanol water, 80 DEG C are extracted 2 hours) The extracting solution obtained afterwards;Wherein edible mushroom is Hericium erinaceus or ganoderma lucidum;
Specifically, the preparation method of high-purity arabinose alcohol of the invention, includes the following steps:
1. 500 molecular weight nanofiltrations;
Edible fungi extract is subjected to nanofiltration operation, pressure control is in 4kg/cm after the column of nanofiltration column2, when material liquid volume subtracts Few, when concentration is promoted, gradually moisturizing dilutes feed liquid to keep membrane flux, (total rate of water make-up and the initial material liquid volume ratio of nanofiltration are 3: 1), isolated to continue reverse osmosis membrane filtration operation less than 500 molecular weight feed liquids;
2. reverse osmosis membrane filtration
Extracting solution less than 500 molecular weight is subjected to reverse osmosis membrane filtration operation, pressure control exists after the column of reverse osmosis membrane 3kg/cm2, filter out water can be used as dilution feed liquid supplement water reuse;
3. crystallizing
Feed liquid is concentrated into its soluble solid content and reaches 50%, dehydrated alcohol is added in 1:5 ratio (volume ratio), It is statically placed at 4 DEG C and crystallizes, filter, obtain coarse crystallization;
4. recrystallizing
Dissolution is heated to after dehydrated alcohol is mixed with the coarse crystallization being collected into, and (coarse crystallization and the weight ratio of dehydrated alcohol are 1:20), it stands, naturally cools to and recrystallize, it is dry after suction filtration, obtain the arabinose alcohol crystals of high-purity.
A kind of preparation method of arabite of the invention has following innovative point:
Preparation method is simple, obtained arabite purity is high, and takes full advantage of the extracting solution of edible mushroom, the present invention The arabite crystallization of high-purity, in addition to this, food can be prepared obtained in process less than 500 molecular weight extracting solutions It can also be used to prepare edible fungi polysaccharide with the surplus materials after bacterium raw material alcohol extracting.
Detailed description of the invention
Fig. 1 arabite chromatography of ions figure
Wherein: 1: antierythrite;2: arabite;3: trehalose;4: mannitol;5: glucose
Specific embodiment
Membrane filter system: the nanofiltration ultra filtering reverse osmosis all-in-one machine of upper sea cowry letter Biotechnology Co., Ltd production, model BH- UF-NF-RO-3-2012;
Filter membrane: Ande Membrane Separation Technology & Engineering (Beijing) Co., Ltd., 500 molecular weight nanofiltration membranes and reverse osmosis membrane, model Respectively NF270 and TW30.
Embodiment 1
1000g ganoderma lucidum (Shanghai Baixin Bio-Technology Co., Ltd.) raw material adds 85% ethyl alcohol successively to extract twice, solid-liquid ratio For 1:15 (weight ratio), extraction is 80 DEG C of temperature, 2 hours each extraction times, and 100 mesh filter cloth mistakes are used after extraction Filter, merges extracting solution twice, the total 15L of obtained extracting solution;
Ethyl alcohol reclaimer operation is carried out under the conditions of 60 DEG C using vacuum concentration instrument first, until fast without ethyl alcohol drop on condenser Until speed flows down, by remainder extracting solution moisturizing to material liquid volume 2L;
2L feed liquid is handled through 500 molecular weight nanofiltrations, and pressure control is in 4kg/cm after the column of 500 molecular weight nanofiltrations2, whenever material Liquid product is reduced to when 1L supplements 1L water into feed liquid to dilute feed concentration again, stops receiving when moisturizing total volume reaches 6L Filter;Being passed through in reverse osmosis separating apparatus less than 500 molecular weight feed liquids for filtering out continues with, and pressure control is in 3kg/cm after column2, When being about 2L to material liquid volume, stop operation.
The reverse osmosis part feed liquid of 500- is collected into about 2L altogether, being concentrated into volume when soluble solid content reaches 50% is Dehydrated alcohol 1500ml is added in 300ml, and (feed liquid and the volume ratio of dehydrated alcohol be 1:5) after mixing, is statically placed in 4 DEG C of rings In border overnight, it is filtered after arabite crystallization is precipitated and obtains the total 25g of coarse crystallization, 500g dehydrated alcohol is added into coarse crystallization (coarse crystallization and the weight ratio of dehydrated alcohol be 1:20), heating stirring dissolve crystallization, are cooled to room temperature, then are placed in weight at 4 DEG C Crystallization, when suction filtration, are rinsed with dehydrated alcohol, after dry, arabinose alcohol crystals are prepared and amount to 21g.
Embodiment 2
The crystallization deionized water dissolving that embodiment 1 is obtained is configured to 10 μ g/ml strength solutions, using it is efficient yin from Sub- chromatography-Pulse amperometric detection method, the ICS-2500 type ion chromatography of Dai An company of reference instrument model U.S. production, with Au For working electrode, Ag/AgCl is reference electrode, pulsed amperometry running parameter: El 100mv, 400ms;E2 is 2000mv, 20ms;E3 is 600mV, 10ms;E4 is 100mV, 70ms.Workstation software is Chromeleon 6.0.Detecting column is The CarboPac MA1 anion-exchange column (4 × 250mm) of Dai An company production, mobile phase are 480mmol/L NaOH, flow velocity 0.40ml/min, applied sample amount 25 μ l, 30 DEG C of column temperature, the arabite standard items and erythrose provided using sigma company Alcohol, mannitol, trehalose, dextrose standard sample are configured to 10 μ g/ml solution as control.
As a result as shown in Figure 1, it can be seen that without other significant sugared peaks, through calculating, the arabinose alcohol crystals of acquisition in sample Purity is 94.5%.
Embodiment 3
1000g Hericium erinaceus (Shanghai Dashanhe Mushroom Technology Co., Ltd.) raw material adds 85% ethyl alcohol successively to extract two Secondary, solid-liquid ratio is 1:15 (weight ratio), and extraction is 80 DEG C of temperature, 2 hours each extraction times, and 100 are used after extraction Mesh filter-cloth filtering merges extracting solution twice, the total 18L of obtained extracting solution;
Ethyl alcohol reclaimer operation is carried out under the conditions of 60 DEG C using vacuum concentration instrument first, until fast without ethyl alcohol drop on condenser Until speed flows down, by remainder extracting solution moisturizing to material liquid volume 2L;
It is handled through 500 molecular weight nanofiltrations, pressure control is in 4kg/cm after the column of 500 molecular weight nanofiltrations2, whenever material liquid volume It is reduced to when 1L and supplements 1L water again into feed liquid to dilute feed concentration, stop nanofiltration when moisturizing total volume reaches 6L;Filter Being passed through in reverse osmosis separating apparatus less than 500 molecular weight feed liquids out continues with, and pressure control is in 3kg/cm after column2, until material When liquid product is about 2L, stop operation.
The reverse osmosis part feed liquid of 500- is collected into about 2L altogether, being concentrated into volume when soluble solid content reaches 50% is Dehydrated alcohol 1800ml is added in 360ml, and (feed liquid and the volume ratio of dehydrated alcohol be 1:5) after mixing, is statically placed in 4 DEG C of rings In border overnight, it is filtered after arabite crystallization is precipitated and obtains the total 30g of coarse crystallization, 600g dehydrated alcohol is added into coarse crystallization (coarse crystallization and the weight ratio of dehydrated alcohol be 1:20), heating stirring dissolve crystallization, are cooled to room temperature, then are placed in weight at 4 DEG C Crystallization, when suction filtration, are rinsed with dehydrated alcohol, after dry, arabinose alcohol crystals are prepared and amount to 25g.
Calculated by detection method used in embodiment 2, the arabite crystal purity of acquisition is 95.3%.

Claims (2)

1. a kind of preparation method of arabite, it is characterised in that this method comprises the following steps:
1. 500 molecular weight nanofiltrations;
Edible fungi extract is carried out to the nanofiltration operation of 500 molecular weight;Collect the part less than 500 molecular weight;
2. reverse osmosis membrane filtration
Extracting solution less than 500 molecular weight is subjected to reverse osmosis membrane filtration operation;
3. crystallizing
Feed liquid is concentrated into its soluble solid content and reaches 40-50%, dehydrated alcohol is added and is crystallized, filters, obtains Coarse crystallization;
4. recrystallizing
It is heated to dissolving after coarse crystallization is mixed with dehydrated alcohol by 1:20 weight ratio, stands, naturally cool to recrystallization, take out It is dry after filter, obtain the sugar alcohol crystal of high-purity;
Wherein, the edible fungi extract is that edible mushroom carries out the extracting solution obtained after alcohol extracting;Wherein edible mushroom is Hericium erinaceus Or ganoderma lucidum.
2. the preparation method of arabite according to claim 1, it is characterised in that include the following steps:
1. 500 molecular weight nanofiltrations;
Edible fungi extract is subjected to nanofiltration operation, pressure control is in 4kg/cm after the column of nanofiltration column2, dense when material liquid volume reduction When degree is promoted, moisturizing dilution feed liquid is isolated to continue reverse osmosis membrane less than 500 molecular weight feed liquids to keep membrane flux Filter operation;
2. reverse osmosis membrane filtration
Extracting solution less than 500 molecular weight is subjected to reverse osmosis membrane filtration operation, pressure control is in 3kg/ after the column of reverse osmosis membrane cm2
3. crystallizing
Feed liquid is concentrated into its soluble solid content and reaches 50%, dehydrated alcohol is added in 1:5 ratio, is statically placed at 4 DEG C Crystallization filters, obtains coarse crystallization;
4. recrystallizing
It is heated to dissolving after dehydrated alcohol is mixed with the coarse crystallization being collected into, the weight ratio of coarse crystallization and dehydrated alcohol is 1: 20, it stands, naturally cools to and recrystallize, dry after suction filtration, obtained arabinose alcohol crystals.
CN201811361361.3A 2018-11-15 2018-11-15 A kind of preparation method of arabite Pending CN109336738A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113004121A (en) * 2021-03-23 2021-06-22 浙江迪萧科技有限公司 High-purity high-yield extraction and purification method of sugar alcohol

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CN105294398A (en) * 2015-09-29 2016-02-03 上海市农业科学院 Method for preparing high-purity mannitol

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN102875330A (en) * 2012-10-16 2013-01-16 广东省农业科学院蚕业与农产品加工研究所 Method for preparing arabitol by flammulina velutipes
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113004121A (en) * 2021-03-23 2021-06-22 浙江迪萧科技有限公司 High-purity high-yield extraction and purification method of sugar alcohol
CN113004121B (en) * 2021-03-23 2022-07-05 浙江迪萧科技有限公司 High-purity high-yield extraction and purification method of sugar alcohol

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