CN107417811B - A kind of inulin method of purification - Google Patents
A kind of inulin method of purification Download PDFInfo
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- CN107417811B CN107417811B CN201710705537.1A CN201710705537A CN107417811B CN 107417811 B CN107417811 B CN 107417811B CN 201710705537 A CN201710705537 A CN 201710705537A CN 107417811 B CN107417811 B CN 107417811B
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- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The invention belongs to food processing technology fields, and in particular to a kind of inulin method of purification.The present invention is handled using the extraction of ultrasonic cell-break Assisted Ethanol, and milk of lime-phosphoric acid method removal of impurities, active carbon decoloring, ion exchange desalination and concentrate drying obtain high-purity inulin.The present invention improves the recovery rate of inulin using the method for ultrasonic wave combination alcohol steep, shortens extraction time, the bioactivity of gained inulin is good, solubility is high.Small using milk of lime-phosphoric acid method removal of impurities loss caused by inulin, impurity treatment is cleaner.And equipment needed for impurity-removing method used in the present invention is simple, and flocculant is at low cost, simple process.Using active carbon decoloring, ion exchange desalination is energy-efficient, without secondary pollution and easy to operate, and products obtained therefrom property is stablized, and purity is high, the degree of polymerization is high, and impurity content is low, and bitter substance is few, and recovery rate is high.
Description
Technical field
The invention belongs to food processing technology fields, and in particular to a kind of inulin method of purification.
Background technique
Inulin also known as synanthrin are a kind of functional levulan from plants such as jerusalem artichoke, witloofs, and most diffluent
Water-soluble dietary fiber.Inulin is nutrition by a state approval in the whole world more than 20 as a kind of pure natural functional ingredient
Enriching substance, be widely used in dairy products, beverage, low-fat low-calorie food, bakery, in health food.Inulin is by D-Fructose
Through chain polysaccharide made of β-(2,1) glucosides key connection, a glucosyl group is often contained in end.The function of inulin includes facilitating
Blood glucose level is controlled, is suitable for diabetes patient, does not cause blood glucose fluctuation；Cholesterol is reduced, blood lipid is controlled, is reduced cardiovascular
The harm of disease；The Bifidobacterium being proliferated in enteron aisle prevents enteric infection；Promote the absorption of minerals；Prevent constipation etc..Inulin
Hygroscopicity is strong, delays moisture to evaporate using this point in food processing, prevents product spoiled, extends Food Shelf-life and guarantees the quality
Phase.
In current inulin method of purification, Hot water extraction often extracts not exclusively during the extraction process, and recovery rate is not high,
The waste of raw material is caused, and water consumption is big, consumed energy higher；There is also energy consumptions in inulin extraction for the adverse current extractive technique of inulin
It is higher, the shortcomings that the high requirements on the equipment.
Summary of the invention
The recovery rate of inulin had can be improved both in order to overcome the above deficiency to provide a kind of inulin method of purification in the present invention,
Energy consumption is reduced again.Steps are as follows for a kind of inulin method of purification of the present invention:
One, feedstock processing: fresh witloof is cleaned, peeling, slice, crush with pulverizer and crosses 120 meshes；
Two, the extraction of ultrasonic cell-break Assisted Ethanol is handled: witloof powder being added in ultrasonic and circulated extraction machine, by certain
80% ethanol water is added in solid-liquid ratio, certain ultrasonic power and at a temperature of carry out ultrasonic and circulated extraction, extraction certain time
Afterwards, it is centrifuged, supernatant is filtered, ultrasonic crude extract is obtained；
Three, removal of impurities is handled: being carried out removal of impurities processing to ultrasonic crude extract using milk of lime-phosphoric acid method, is obtained removal of impurities liquid；
Four, decolorization: decolorization is carried out to removal of impurities liquid using active carbon, obtains destainer；
Five, desalting processing: desalting processing is carried out to destainer using ion exchange, obtains desalinization liquor；
Six, it is concentrated and dried: by desalinization liquor concentration, drying, obtaining high-purity inulin.
Solid-liquid ratio described in step 2 is 1:5-10, and the ultrasonic power is 400-600W, and the ultrasonic temperature is 30-50
DEG C, the extraction time is 20-40min.
The processing of removal of impurities described in step 3 is that the pH value of ultrasonic crude extract is adjusted to 10-12 with milk of lime, in 40-60 DEG C of temperature
Lower processing 5-10min is filtered, and phosphoric acid is added into filtrate and pH is adjusted to 6.0, in 70 DEG C of heat preservation 30min, is filtered, is removed
Miscellaneous liquid.
During decolorization described in step 4, activated carbon dosage 0.5-0.7g/100mL, bleaching temperature 60-75
DEG C, bleaching time 20-30min.
In desalting processing ion exchange process described in step 5, destainer is with 2-5mL/min by being equipped with LSA-21 resin
Ion exchange column obtain desalinization liquor in 15-30 DEG C of Dynamic Adsorption 4h of temperature.
Condition is concentrated described in step 6 are as follows: vacuum degree 0.07MPa, temperature are 65 DEG C, and 6min is concentrated.
Drying condition described in step 6 are as follows: 180 DEG C of drying temperature, drying time 16s.
The present invention uses ultrasonic cell-break Assisted Ethanol leach extraction method, is generated using ultrasonic wave to witloof unique
Mechanical oscillation effect and cavitation destroy the cell wall structure of witloof, make its cell wall rupture, discharge intracellular effective
Ingredient makes inulin be directly entered solvent and is sufficiently mixed, to improve the recovery rate of inulin.Meanwhile the present invention is using ultrasound
The method of wave combination alcohol steep shortens extraction time, and the bioactivity of gained inulin is good, solubility is high.
The present invention, which carries out removal of impurities to inulin crude extract using milk of lime-phosphoric acid method, to be neutralized in crude extract using milk of lime
Organic acid, adjust back pH with phosphoric acid later, while generating the flocculent deposit of a large amount of complicated components, remove protein in solution,
The impurity such as cellulose, pectin.Since Inulin polysaccharide has exceeded the adsorption capacity of floccule, removed using milk of lime-phosphoric acid method
The miscellaneous loss caused by inulin is small, and impurity treatment is cleaner.And equipment needed for impurity-removing method used in the present invention is simple, flocculation
Agent is at low cost, simple process.
The present invention is energy-efficient using active carbon decolorization, the method for ion exchange desalting processing, without secondary pollution, and
Easy to operate, products obtained therefrom property is stablized, and purity is high, the degree of polymerization is high, and impurity content is low, and bitter substance is few, and recovery rate is high.
Specific embodiment
Below with reference to embodiment, the following further describes the technical solution of the present invention, and however, it is not limited to this, all right
Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be contained
Lid is within the protection scope of the present invention.
Embodiment 1
A kind of inulin method of purification, steps are as follows:
One, feedstock processing: fresh witloof is cleaned, peeling, slice, crush with pulverizer and crosses 120 meshes；
Two, the extraction of ultrasonic cell-break Assisted Ethanol is handled: witloof powder being added in ultrasonic and circulated extraction machine, by feed liquid
Than 80% ethanol water is added for 1:7, ultrasonic and circulated extraction is carried out at a temperature of 500W ultrasonic power and 40 DEG C, is extracted
After 30min, centrifugation filters supernatant, obtains ultrasonic crude extract, inulin recovery rate reaches 85.7%.
Three, removal of impurities is handled: the pH value of ultrasonic crude extract is adjusted to 11 using milk of lime, handles 8min at 50 °C,
It filters, phosphoric acid is added into filtrate and pH is adjusted to 6.0, in 70 DEG C of heat preservation 30min, filter, obtain removal of impurities liquid.
Phosphoric acid is added in calcium hydroxide, originally generates precipitating, and most total precipitating disappears, therefore the additional amount of phosphoric acid needs to control
It is good.When the quality that phosphoric acid is added is 0.88-1.32 times of calcium hydroxide, all calcium ions precipitates can be made to fall.
Four, decolorization: decolorization is carried out to removal of impurities liquid using active carbon, activated carbon dosage 0.6g/100mL takes off
Color temperature is 70 DEG C, bleaching time 25min.Destainer is obtained, light transmittance reaches 95%；
Five, desalting processing: carrying out desalting processing to destainer using ion exchange, in ion exchange process, destainer with
3mL/min obtains desalinization liquor in 30 DEG C of Dynamic Adsorption 4h of temperature by the ion exchange column equipped with LSA-21 resin；
Six, it being concentrated and dried: desalinization liquor concentrate drying is handled, concentration condition is vacuum degree 0.07MPa, and temperature is 65 DEG C,
6min is concentrated；Drying condition is 180 DEG C of drying temperature, and drying time 16s obtains high-purity inulin, through detecting inulin purity
Reach 93.5%, based on raw material solid content, inulin recovery rate is 76.4%.
Embodiment 2
A kind of inulin method of purification, steps are as follows:
One, feedstock processing: fresh witloof is cleaned, peeling, slice, crush with pulverizer and crosses 120 meshes；
Two, the extraction of ultrasonic cell-break Assisted Ethanol is handled: witloof powder being added in ultrasonic and circulated extraction machine, by feed liquid
Than 80% ethanol water is added for 1:6, ultrasonic and circulated extraction is carried out at a temperature of 400W ultrasonic power and 30 DEG C, is extracted
After 40min, centrifugation filters supernatant, obtains ultrasonic crude extract, inulin recovery rate reaches 84.3%.
Three, removal of impurities is handled: the pH value of ultrasonic crude extract is adjusted to 10 using milk of lime, handles 6min at a temperature of 40 DEG C,
It filters, phosphoric acid is added into filtrate, in 70 DEG C of heat preservation 30min after pH is adjusted to 6.0, filter, obtained clarified solution is removal of impurities liquid.
Four, decolorization: decolorization is carried out to removal of impurities liquid using active carbon, activated carbon dosage 0.5g/100mL takes off
Color temperature is 60 DEG C, bleaching time 30min.Destainer is obtained, light transmittance reaches 94.6%；
Five, desalting processing: carrying out desalting processing to destainer using ion exchange, in ion exchange process, destainer with
2mL/min obtains desalinization liquor in 15 DEG C of Dynamic Adsorption 4h of temperature by the ion exchange column equipped with LSA-21 resin；
Six, it being concentrated and dried: desalinization liquor concentrate drying is handled, concentration condition is vacuum degree 0.07MPa, and temperature is 65 DEG C,
6min is concentrated；Drying condition is 180 DEG C of drying temperature, and drying time 16s obtains high-purity inulin, through detecting inulin purity
Reach 92.8%, based on raw material solid content, inulin recovery rate is 72.7%.
Embodiment 3
A kind of inulin method of purification, steps are as follows:
One, feedstock processing: fresh witloof is cleaned, peeling, slice, crush with pulverizer and crosses 120 meshes；
Two, the extraction of ultrasonic cell-break Assisted Ethanol is handled: witloof powder being added in ultrasonic and circulated extraction machine, by feed liquid
Than 80% ethanol water is added for 1:5, ultrasonic and circulated extraction is carried out at a temperature of 600W ultrasonic power and 50 DEG C, is extracted
After 30min, centrifugation filters supernatant, obtains ultrasonic crude extract, inulin recovery rate reaches 82.8%.
Three, removal of impurities is handled: the pH value of ultrasonic crude extract is adjusted to 12 using milk of lime, handles 7min at a temperature of 60 DEG C,
It filters, phosphoric acid is added into filtrate, in 70 DEG C of heat preservation 30min after pH is adjusted to 6.0, filter, obtained clarified solution is removal of impurities liquid.
Four, decolorization: decolorization is carried out to removal of impurities liquid using active carbon, activated carbon dosage 0.7g/100mL takes off
Color temperature is 65 DEG C, bleaching time 23min.Destainer is obtained, light transmittance reaches 93%；
Five, desalting processing: carrying out desalting processing to destainer using ion exchange, in ion exchange process, destainer with
4mL/min obtains desalinization liquor in 20 DEG C of Dynamic Adsorption 4h of temperature by the ion exchange column equipped with LSA-21 resin；
Six, it being concentrated and dried: desalinization liquor concentrate drying is handled, concentration condition is vacuum degree 0.07MPa, and temperature is 65 DEG C,
6min is concentrated；Drying condition is 180 DEG C of drying temperature, and drying time 16s obtains high-purity inulin, through detecting inulin purity
Reach 92.1%, based on raw material solid content, inulin recovery rate is 71.3%.
Embodiment 4
A kind of inulin method of purification, steps are as follows:
One, feedstock processing: fresh witloof is cleaned, peeling, slice, crush with pulverizer and crosses 120 meshes；
Two, the extraction of ultrasonic cell-break Assisted Ethanol is handled: witloof powder being added in ultrasonic and circulated extraction machine, by feed liquid
Than 80% ethanol water is added for 1:8, ultrasonic and circulated extraction is carried out at a temperature of 500W ultrasonic power and 40 DEG C, is extracted
After 20min, centrifugation filters supernatant, obtains ultrasonic crude extract, inulin recovery rate reaches 84.7%.
Three, removal of impurities is handled: the pH value of ultrasonic crude extract is adjusted to 11 using milk of lime, handles 9min at a temperature of 40 DEG C,
It filters, phosphoric acid is added into filtrate, in 70 DEG C of heat preservation 30min after pH is adjusted to 6.0, filter, obtained clarified solution is removal of impurities liquid.
Four, decolorization: decolorization is carried out to removal of impurities liquid using active carbon, activated carbon dosage 0.5g/100mL takes off
Color temperature is 75 DEG C, bleaching time 28min.Destainer is obtained, light transmittance reaches 94.7%；
Five, desalting processing: carrying out desalting processing to destainer using ion exchange, in ion exchange process, destainer with
5mL/min obtains desalinization liquor in 25 DEG C of Dynamic Adsorption 4h of temperature by the ion exchange column equipped with LSA-21 resin；
Six, it being concentrated and dried: desalinization liquor concentrate drying is handled, concentration condition is vacuum degree 0.07MPa, and temperature is 65 DEG C,
6min is concentrated；Drying condition is 180 DEG C of drying temperature, and drying time 16s obtains high-purity inulin, through detecting inulin purity
Reach 90.5%, based on raw material solid content, inulin recovery rate is 73.6%.
Comparative example 1: steps are as follows for heating restricted-access media inulin:
One, feedstock processing: fresh witloof is cleaned, peeling, slice, crush with pulverizer and crosses 120 meshes；
Two, heating extraction: pot for solvent extraction is added in inulin, 80 DEG C of temperature, 90min is stirred and evenly mixed, obtains inulin leaching liquor, chrysanthemum
Powder recovery rate reaches 75.3%；
Three, removal of impurities is handled: the pH value of inulin leaching liquor is adjusted to 10 using milk of lime, handles 6min at a temperature of 40 DEG C,
It filters, phosphoric acid is added into filtrate, in 70 DEG C of heat preservation 30min after pH is adjusted to 6.0, filter, obtained clarified solution is removal of impurities liquid.
Four, decolorization: decolorization is carried out to removal of impurities liquid using active carbon, activated carbon dosage 0.5g/100mL takes off
Color temperature is 60 DEG C, bleaching time 30min.Destainer is obtained, light transmittance reaches 90%；
Five, desalting processing: carrying out desalting processing to destainer using ion exchange, in ion exchange process, destainer with
2mL/min obtains desalinization liquor in 15 DEG C of Dynamic Adsorption 4h of temperature by the ion exchange column equipped with LSA-21 resin；
Six, it being concentrated and dried: desalinization liquor concentrate drying is handled, concentration condition is vacuum degree 0.07MPa, and temperature is 65 DEG C,
6min is concentrated；Drying condition is 180 DEG C of drying temperature, drying time 16s, obtains purifying inulin, is detected inulin purity and is
89%, based on raw material solid content, inulin recovery rate is 52.3%.
Claims (6)
1. a kind of inulin method of purification, it is characterised in that the method comprises the following steps:
One, feedstock processing: fresh witloof is cleaned, peeling, slice, crush with pulverizer and crosses 120 meshes；
Two, the extraction of ultrasonic cell-break Assisted Ethanol is handled: witloof powder is added in ultrasonic and circulated extraction machine, by solid-liquid ratio 1:
80% ethanol water is added in 5-10, and ultrasonic and circulated extraction is carried out at a temperature of 400-600W ultrasonic power and 30-50 DEG C, extracts
After 20-40min, centrifugation filters supernatant, obtains ultrasonic crude extract；
Three, removal of impurities is handled: being carried out removal of impurities processing to ultrasonic crude extract using milk of lime-phosphoric acid method, is obtained removal of impurities liquid；
Four, decolorization: decolorization is carried out to removal of impurities liquid using active carbon, obtains destainer；
Five, desalting processing: desalting processing is carried out to destainer using ion exchange, obtains desalinization liquor；
Six, it is concentrated and dried: by desalinization liquor concentration, drying, obtaining high-purity inulin.
2. a kind of inulin method of purification according to claim 1, it is characterised in that the processing of removal of impurities described in step 3 is to use lime
The pH value of ultrasonic crude extract is adjusted to 10-12 by cream, and 5-10min is handled at a temperature of 40-60 DEG C, filters, phosphorus is added into filtrate
PH is simultaneously adjusted to 6.0 by acid, in 70 DEG C of heat preservation 30min, is filtered, and removal of impurities liquid is obtained.
3. a kind of inulin method of purification according to claim 1, it is characterised in that living during decolorization described in step 4
Property charcoal dosage be 0.5-0.7g/100mL, bleaching temperature be 60-75 DEG C, bleaching time 20-30min.
4. a kind of inulin method of purification according to claim 1, it is characterised in that desalting processing ion exchange described in step 5
In the process, destainer with 2-5mL/min by be equipped with LSA-21 resin ion exchange column, in 15-30 DEG C of Dynamic Adsorption of temperature
4h obtains desalinization liquor.
5. a kind of inulin method of purification according to claim 1, it is characterised in that condition is concentrated described in step 6 are as follows: vacuum degree
0.07MPa, temperature are 65 DEG C, and 6min is concentrated.
6. a kind of inulin method of purification according to claim 1, it is characterised in that drying condition described in step 6 are as follows: dry temperature
180 DEG C of degree, drying time 16s.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108467441A (en) * | 2018-04-25 | 2018-08-31 | 厦门欣赛科技有限公司 | A kind of inulin preparation method and preparation system |
| CN110527001A (en) * | 2019-09-24 | 2019-12-03 | 武汉轻工大学 | A kind of witloof polysaccharide and its extraction process and application |
| CN110981994A (en) * | 2019-12-24 | 2020-04-10 | 陕西森弗天然制品有限公司 | Method for extracting high-purity inulin |
| CN114946909B (en) * | 2021-12-16 | 2023-08-29 | 中国人民解放军空军特色医学中心 | Wafer biscuit with obesity relieving effect |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965377A (en) * | 2014-05-14 | 2014-08-06 | 东南大学 | Method for preparing synanthrin from jerusalem artichoke |
| CN104059158A (en) * | 2014-06-17 | 2014-09-24 | 熊鹏 | Leaching method of alantin |
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- 2017-08-16 CN CN201710705537.1A patent/CN107417811B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965377A (en) * | 2014-05-14 | 2014-08-06 | 东南大学 | Method for preparing synanthrin from jerusalem artichoke |
| CN104059158A (en) * | 2014-06-17 | 2014-09-24 | 熊鹏 | Leaching method of alantin |
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