CN107417811A - A kind of inulin method of purification - Google Patents
A kind of inulin method of purification Download PDFInfo
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- CN107417811A CN107417811A CN201710705537.1A CN201710705537A CN107417811A CN 107417811 A CN107417811 A CN 107417811A CN 201710705537 A CN201710705537 A CN 201710705537A CN 107417811 A CN107417811 A CN 107417811A
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- 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 field, 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, the removal of impurities of milk of lime phosphoric acid method, activated carbon decolorizing, and 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, and the bioactivity of gained inulin is good, solubility is high.Using the removal of impurities of milk of lime phosphoric acid method, the loss to caused by inulin is small, and impurity treatment is cleaner.And equipment is simple needed for impurity-removing method used in the present invention, flocculant cost is low, and technique is simple.Using activated carbon decolorizing, ion exchange desalination efficient energy-saving, non-secondary pollution, and easily operation, products obtained therefrom property is stable, and purity is high, and 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 field, and in particular to a kind of inulin method of purification.
Background technology
Inulin, also known as synanthrin, it is a kind of feature levulan from plants such as jerusalem artichoke, witloofs, and it is most diffluent
Water-soluble dietary fiber.Inulin is nutrition by more than 20 individual state approval of the whole world as a kind of pure natural functional ingredient
Enriching substance, it is widely used in dairy products, beverage, low-fat low-calorie food, bakery, health food.Inulin is by D-Fructose
Through β-the chain polysaccharide that is formed by connecting of (2,1) glycosidic bond, a glucosyl group is often contained in end.The function of inulin includes contributing to
Blood sugar level is controlled, is suitable for diabetes patient, does not cause blood glucose fluctuation；Cholesterol is reduced, controls blood fat, is reduced cardiovascular
The harm of disease；Breed the Bifidobacterium in enteron aisle, prevent enteric infection；Promote the absorption of mineral matter；Prevent constipation etc..Inulin
Hygroscopicity is strong, delays moisture evaporation using this point in food processing, prevents that product is spoiled, extends Food Shelf-life and guarantees the quality
Phase.
In current inulin method of purification, often extraction is incomplete in extraction process for Hot water extraction, and recovery rate is not high,
The waste of raw material is caused, and water consumption is big, and power consumption is higher；There is also energy consumption in inulin extraction for the adverse current extractive technique of inulin
It is higher, it is high to equipment requirement the shortcomings that.
The content of the invention
The present invention can both improve the recovery rate of inulin to overcome above deficiency to provide a kind of inulin method of purification,
Energy consumption is reduced again.A kind of inulin method of purification step of the present invention is as follows：
First, Feedstock treating：By fresh witloof through cleaning, removing the peel, section, crushed with pulverizer and cross 120 mesh sieves；
2nd, the extraction of ultrasonic cell-break Assisted Ethanol is handled：Witloof powder is added in ultrasonic and circulated extraction machine, by certain
Solid-liquid ratio adds 80% ethanol water, and ultrasonic and circulated extraction is carried out with a temperature of in certain ultrasonic power, extracts certain time
Afterwards, centrifuge, supernatant is filtered, obtains ultrasonic crude extract；
3rd, removal of impurities is handled：Removal of impurities processing is carried out to ultrasonic crude extract using milk of lime-phosphoric acid method, obtains the liquid that cleans；
4th, decolorization：Decolorization is carried out to removal of impurities liquid using activated carbon, obtains destainer；
5th, desalting processing：Desalting processing is carried out to destainer using ion exchange, obtains desalinization liquor；
6th, it is concentrated and dried：Desalinization liquor is concentrated, dried, obtains high-purity inulin.
Solid-liquid ratio described in step 2 is 1:5-10, the ultrasonic power are 400-600W, and the ultrasonic temperature is 30-50
DEG C, the extraction time is 20-40min.
Removal of impurities processing is that the pH value of ultrasonic crude extract is adjusted into 10-12 with milk of lime described in step 3, in 40-60 DEG C of temperature
Lower processing 5-10min, filter, phosphoric acid is added into filtrate and pH is adjusted to 6.0, be incubated 30min at 70 DEG C, filter, 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 passed through equipped with LSA-21 resins with 2-5mL/min
Ion exchange column, in 15-30 DEG C of Dynamic Adsorption 4h of temperature, obtain desalinization liquor.
Condition is concentrated described in step 6 is：Vacuum 0.07MPa, temperature are 65 DEG C, concentrate 6min.
Drying condition is described in step 6：180 DEG C of drying temperature, drying time 16s.
The present invention uses ultrasonic cell-break Assisted Ethanol leach extraction method, using ultrasonic wave to unique caused by witloof
Mechanical oscillation effect and cavitation, the cell wall structure of witloof is destroyed, make its cell wall rupture, discharged intracellular effective
Composition, inulin is directly entered solvent and be sufficiently mixed, so as to improve the recovery rate of inulin.Meanwhile the present invention is using ultrasound
The method of ripple combination alcohol steep, shortens extraction time, and the bioactivity of gained inulin is good, solubility is high.
It is to be neutralized using milk of lime in crude extract that the present invention carries out removal of impurities to inulin crude extract using milk of lime-phosphoric acid method
Organic acid, adjust back pH with phosphoric acid afterwards, while produce the flocculent deposit of a large amount of complicated components, remove protein in solution,
The impurity such as cellulose, pectin.Removed because Inulin polysaccharide is beyond the adsorption capacity of floccule, therefore using milk of lime-phosphoric acid method
The miscellaneous loss to caused by inulin is small, and impurity treatment is cleaner.And equipment is simple needed for impurity-removing method used in the present invention, flocculation
Agent cost is low, and technique is simple.
The present invention is handled using activated carbon decolorizing, the method efficient energy-saving of ion exchange desalting processing, non-secondary pollution, and
Easily operation, products obtained therefrom property is stable, and purity is high, and the degree of polymerization is high, and impurity content is low, and bitter substance is few, and recovery rate is high.
Embodiment
Technical scheme is described further with reference to embodiment, but is not limited thereto, it is every right
Technical solution of the present invention is modified or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, all should contain
Cover in protection scope of the present invention.
Embodiment 1
A kind of inulin method of purification, step are as follows：
First, Feedstock treating：By fresh witloof through cleaning, removing the peel, section, crushed with pulverizer and cross 120 mesh sieves；
2nd, the extraction of ultrasonic cell-break Assisted Ethanol is handled：Witloof powder is added in ultrasonic and circulated extraction machine, by feed liquid
Than for 1:7 add 80% ethanol water, and ultrasonic and circulated extraction is carried out at a temperature of 500W ultrasonic powers and 40 DEG C, extract
After 30min, centrifugation, supernatant is filtered, obtains ultrasonic crude extract, inulin extraction rate reached to 85.7%.
3rd, removal of impurities is handled：The pH value of ultrasonic crude extract is adjusted to 11 using milk of lime, 8min is handled at a temperature of 50 DEG C,
Filter, phosphoric acid is added into filtrate and pH is adjusted to 6.0, be incubated 30min at 70 DEG C, filter, obtain the liquid that cleans.
Phosphoric acid is added in calcium hydroxide, originally produces precipitation, and most total precipitation disappears, therefore the addition of phosphoric acid needs to control
It is good.It when the quality that phosphoric acid adds is 0.88-1.32 times of calcium hydroxide, can fall all calcium ions precipitates.
4th, decolorization：Decolorization is carried out to removal of impurities liquid using activated carbon, activated carbon dosage 0.6g/100mL, taken off
Color temperature is 70 DEG C, bleaching time 25min.Destainer is obtained, light transmittance reaches 95%；
5th, desalting processing：Desalting processing is carried out to destainer using ion exchange, in ion exchange process, destainer with
3mL/min, in 30 DEG C of Dynamic Adsorption 4h of temperature, obtains desalinization liquor by the ion exchange column equipped with LSA-21 resins；
6th, it is concentrated and dried：Desalinization liquor concentrate drying is handled, concentration condition is vacuum 0.07MPa, and temperature is 65 DEG C,
Concentrate 6min；Drying condition is 180 DEG C of drying temperature, drying time 16s, to obtain high-purity inulin, after testing 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, step are as follows：
First, Feedstock treating：By fresh witloof through cleaning, removing the peel, section, crushed with pulverizer and cross 120 mesh sieves；
2nd, the extraction of ultrasonic cell-break Assisted Ethanol is handled：Witloof powder is added in ultrasonic and circulated extraction machine, by feed liquid
Than for 1:6 add 80% ethanol water, and ultrasonic and circulated extraction is carried out at a temperature of 400W ultrasonic powers and 30 DEG C, extract
After 40min, centrifugation, supernatant is filtered, obtains ultrasonic crude extract, inulin extraction rate reached to 84.3%.
3rd, removal of impurities is handled：The pH value of ultrasonic crude extract is adjusted to 10 using milk of lime, 6min is handled at a temperature of 40 DEG C,
Filter, phosphoric acid is added into filtrate, 30min is incubated at 70 DEG C after pH is adjusted into 6.0, filter, obtained clarified solution is removal of impurities liquid.
4th, decolorization：Decolorization is carried out to removal of impurities liquid using activated carbon, activated carbon dosage 0.5g/100mL, taken off
Color temperature is 60 DEG C, bleaching time 30min.Destainer is obtained, light transmittance reaches 94.6%；
5th, desalting processing：Desalting processing is carried out to destainer using ion exchange, in ion exchange process, destainer with
2mL/min, in 15 DEG C of Dynamic Adsorption 4h of temperature, obtains desalinization liquor by the ion exchange column equipped with LSA-21 resins；
6th, it is concentrated and dried：Desalinization liquor concentrate drying is handled, concentration condition is vacuum 0.07MPa, and temperature is 65 DEG C,
Concentrate 6min；Drying condition is 180 DEG C of drying temperature, drying time 16s, to obtain high-purity inulin, after testing 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, step are as follows：
First, Feedstock treating：By fresh witloof through cleaning, removing the peel, section, crushed with pulverizer and cross 120 mesh sieves；
2nd, the extraction of ultrasonic cell-break Assisted Ethanol is handled：Witloof powder is added in ultrasonic and circulated extraction machine, by feed liquid
Than for 1:5 add 80% ethanol water, and ultrasonic and circulated extraction is carried out at a temperature of 600W ultrasonic powers and 50 DEG C, extract
After 30min, centrifugation, supernatant is filtered, obtains ultrasonic crude extract, inulin extraction rate reached to 82.8%.
3rd, removal of impurities is handled：The pH value of ultrasonic crude extract is adjusted to 12 using milk of lime, 7min is handled at a temperature of 60 DEG C,
Filter, phosphoric acid is added into filtrate, 30min is incubated at 70 DEG C after pH is adjusted into 6.0, filter, obtained clarified solution is removal of impurities liquid.
4th, decolorization：Decolorization is carried out to removal of impurities liquid using activated carbon, activated carbon dosage 0.7g/100mL, taken off
Color temperature is 65 DEG C, bleaching time 23min.Destainer is obtained, light transmittance reaches 93%；
5th, desalting processing：Desalting processing is carried out to destainer using ion exchange, in ion exchange process, destainer with
4mL/min, in 20 DEG C of Dynamic Adsorption 4h of temperature, obtains desalinization liquor by the ion exchange column equipped with LSA-21 resins；
6th, it is concentrated and dried：Desalinization liquor concentrate drying is handled, concentration condition is vacuum 0.07MPa, and temperature is 65 DEG C,
Concentrate 6min；Drying condition is 180 DEG C of drying temperature, drying time 16s, to obtain high-purity inulin, after testing 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, step are as follows：
First, Feedstock treating：By fresh witloof through cleaning, removing the peel, section, crushed with pulverizer and cross 120 mesh sieves；
2nd, the extraction of ultrasonic cell-break Assisted Ethanol is handled：Witloof powder is added in ultrasonic and circulated extraction machine, by feed liquid
Than for 1:8 add 80% ethanol water, and ultrasonic and circulated extraction is carried out at a temperature of 500W ultrasonic powers and 40 DEG C, extract
After 20min, centrifugation, supernatant is filtered, obtains ultrasonic crude extract, inulin extraction rate reached to 84.7%.
3rd, removal of impurities is handled：The pH value of ultrasonic crude extract is adjusted to 11 using milk of lime, 9min is handled at a temperature of 40 DEG C,
Filter, phosphoric acid is added into filtrate, 30min is incubated at 70 DEG C after pH is adjusted into 6.0, filter, obtained clarified solution is removal of impurities liquid.
4th, decolorization：Decolorization is carried out to removal of impurities liquid using activated carbon, activated carbon dosage 0.5g/100mL, taken off
Color temperature is 75 DEG C, bleaching time 28min.Destainer is obtained, light transmittance reaches 94.7%；
5th, desalting processing：Desalting processing is carried out to destainer using ion exchange, in ion exchange process, destainer with
5mL/min, in 25 DEG C of Dynamic Adsorption 4h of temperature, obtains desalinization liquor by the ion exchange column equipped with LSA-21 resins；
6th, it is concentrated and dried：Desalinization liquor concentrate drying is handled, concentration condition is vacuum 0.07MPa, and temperature is 65 DEG C,
Concentrate 6min；Drying condition is 180 DEG C of drying temperature, drying time 16s, to obtain high-purity inulin, after testing inulin purity
Reach 90.5%, based on raw material solid content, inulin recovery rate is 73.6%.
Comparative example 1：It is as follows to heat restricted-access media inulin step：
First, Feedstock treating：By fresh witloof through cleaning, removing the peel, section, crushed with pulverizer and cross 120 mesh sieves；
2nd, heating extraction：Inulin is added into pot for solvent extraction, 80 DEG C of temperature, 90min is stirred and evenly mixed, obtains inulin leaching liquor, chrysanthemum
Powder extraction rate reached is to 75.3%；
3rd, removal of impurities is handled：The pH value of inulin leaching liquor is adjusted to 10 using milk of lime, 6min is handled at a temperature of 40 DEG C,
Filter, phosphoric acid is added into filtrate, 30min is incubated at 70 DEG C after pH is adjusted into 6.0, filter, obtained clarified solution is removal of impurities liquid.
4th, decolorization：Decolorization is carried out to removal of impurities liquid using activated carbon, activated carbon dosage 0.5g/100mL, taken off
Color temperature is 60 DEG C, bleaching time 30min.Destainer is obtained, light transmittance reaches 90%；
5th, desalting processing：Desalting processing is carried out to destainer using ion exchange, in ion exchange process, destainer with
2mL/min, in 15 DEG C of Dynamic Adsorption 4h of temperature, obtains desalinization liquor by the ion exchange column equipped with LSA-21 resins；
6th, it is concentrated and dried：Desalinization liquor concentrate drying is handled, concentration condition is vacuum 0.07MPa, and temperature is 65 DEG C,
Concentrate 6min；Drying condition is 180 DEG C, drying time 16s of drying temperature, obtains purifying inulin, inulin purity is after testing
89%, based on raw material solid content, inulin recovery rate is 52.3%.
Claims (7)
1. a kind of inulin method of purification, it is characterised in that methods described step is as follows：
First, Feedstock treating：By fresh witloof through cleaning, removing the peel, section, crushed with pulverizer and cross 120 mesh sieves；
2nd, the extraction of ultrasonic cell-break Assisted Ethanol is handled：Witloof powder is added in ultrasonic and circulated extraction machine, by certain feed liquid
Than adding 80% ethanol water, ultrasonic and circulated extraction is carried out with a temperature of in certain ultrasonic power, after extracting certain time, from
The heart, supernatant is filtered, obtain ultrasonic crude extract；
3rd, removal of impurities is handled：Removal of impurities processing is carried out to ultrasonic crude extract using milk of lime-phosphoric acid method, obtains the liquid that cleans；
4th, decolorization：Decolorization is carried out to removal of impurities liquid using activated carbon, obtains destainer；
5th, desalting processing：Desalting processing is carried out to destainer using ion exchange, obtains desalinization liquor；
6th, it is concentrated and dried：Desalinization liquor is concentrated, dried, obtains high-purity inulin.
2. a kind of inulin method of purification according to claim 1, it is characterised in that solid-liquid ratio described in step 2 is 1:5-10, institute
It is 400-600W to state ultrasonic power, and the ultrasonic temperature is 30-50 DEG C, and the extraction time is 20-40min.
3. a kind of inulin method of purification according to claim 1, it is characterised in that removal of impurities processing is to use lime described in step 3
The pH value of ultrasonic crude extract is adjusted to 10-12 by breast, 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, is incubated 30min at 70 DEG C, is filtered, obtains the liquid that cleans.
4. 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.
A kind of 5. inulin method of purification according to claim 1, it is characterised in that desalting processing ion exchange described in step 5
During, destainer with 2-5mL/min by the ion exchange column equipped with LSA-21 resins, in 15-30 DEG C of Dynamic Adsorption of temperature
4h, obtain desalinization liquor.
6. a kind of inulin method of purification according to claim 1, it is characterised in that concentration condition is described in step 6：Vacuum
0.07MPa, temperature are 65 DEG C, concentrate 6min.
7. a kind of inulin method of purification according to claim 1, it is characterised in that drying condition is described in step 6：Dry temperature
180 DEG C of degree, drying time 16s.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114946909A (en) * | 2021-12-16 | 2022-08-30 | 中国人民解放军空军特色医学中心 | Wafer biscuit with effect of relieving obesity |
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 |
-
2017
- 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 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114946909A (en) * | 2021-12-16 | 2022-08-30 | 中国人民解放军空军特色医学中心 | Wafer biscuit with effect of relieving obesity |
| 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 |
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