CN104151445B - A kind of method extracting natural low methoxyl pectin from sunflower plate - Google Patents
A kind of method extracting natural low methoxyl pectin from sunflower plate Download PDFInfo
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- CN104151445B CN104151445B CN201410190823.5A CN201410190823A CN104151445B CN 104151445 B CN104151445 B CN 104151445B CN 201410190823 A CN201410190823 A CN 201410190823A CN 104151445 B CN104151445 B CN 104151445B
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Abstract
A kind of method extracting natural low methoxyl pectin from sunflower plate, its step includes: wash, extract, ultrafiltration desalination, ion exchange removing remaining salinity, spray drying, reverse osmosis, recovery calcium citrate.Wherein extracting chelating agen used is sodium citrate, and concentration is 0.4～1.0% (sodium citrate: water), and extracting solid-to-liquid ratio is 1: 20～1: 50 (sunflower plate dry powder: water), and by pH regulator to 2～4；Afterwards with the ultrafilter membrane removing major part salinity of molecular cut off 5000～10000Da, remove remaining salinity with ion exchange.It is an advantage of the current invention that pectin extraction rate can reach 10～15% (based on galacturonic acid, to raw material), ultrafiltration desalination can remove the salinity of more than 90%, the low methoxyl pectin esterification degree prepared is 25～30%, amidation degree is 3～10%, galacturonic acid content 65～80% (to pectin), weight average molecular weight 200～300kDa.Sodium citrate has very high security as chelating agen, adds calcium hydroxide and can realize reclaiming calcium citrate after reverse osmosis.
Description
Technical field
The invention belongs to food colloid field, extract the preparation method of the natural low methoxyl pectin combining ultrafiltration purification particularly to a kind of novel chelating agents.
Background technology
Pectin is a kind of labyrinth polysaccharide being widely present in terrestrial plant cell wall.Add at food such as bakery, acidic milk drink, fruit juice
In work, pectin, as hydrophilic colloid, has the effects such as gelling, stable and thickening.Meanwhile, pectin is also natural water soluble dietary fiber, has
Regulation human body intestinal canal microenvironment, reduces the beneficial functionals such as blood fat.
Pectin can be divided into high-esterpectin (esterification degree ＞ 50%) and low methoxyl pectin (esterification degree ＜ 50%).Business pectin mostly is high-esterpectin at present, and it is former
Material predominantly Fructus Citri tangerinae section fruit skin slag, apple peel and Radix Betae skin slag etc..Low methoxyl pectin as stabilizer, gel and thickening agent can unique application in
Low sugar, low-calorie functionality food, on the fruit jam of low sugar, fruit jelly, soft sweet, frozen confection, ice cream, Yoghourt sarcocarp bed material, baked goods
The production of light etc..The at present whole world low methoxyl pectin market demand about 5000 tons/year, and with 10～the speed increase of 20%.Pectin in sunflower plate is i.e.
For natural low methoxyl pectin, China's sunflower planting area reaches 960000m2, contain abundant natural low methoxyl pectin resource.
After current industrial pectin extraction method is mainly acidity extraction, then precipitate with ethanol, i.e. utilize acid hydrolysis cell wall to discharge pectin, afterwards profit
Realize pectin by the pectin characteristic insoluble in alcohol to separate with other materials.Wherein, acidity extraction is commonly incorporated into disodiumedetate, phosphate,
The chelating agen assisted extraction such as ammonium oxalate, but pectin post processing cost can be improved and cause security risk；Ethanol precipitation process need to expend a large amount of ethanol, makes
One-tenth recovery energy consumption is big, environment protection treating high in cost of production problem.Pectin is entered by the Physical Separation Technology that therefore, it can be considered as the safely cleanings such as membrance separation
Row is isolated and purified.
Summary of the invention
It is an object of the invention to provide a kind of industrialization, safe and simple natural low methoxyl pectin technology of preparing of being prone to, use sodium citrate to extract combination super
The method of filter purification extracts pectin, while obtaining high extraction and high purity product, improves Product Safety, reduces production cost, eliminates
Environmental issue.
The principle of the present invention is: natural pectin and Ca2+Form chelation structure, be unfavorable for pectin extraction.Sodium citrate can be captured and fruit as chelating agen
The Ca of complexation in glue2+, promote that pectin is soluble in water；Regulation reaction pH be 2～4 can cellulose in partial hydrolysis cell wall and hemicellulose, have
Profit pectin dissolution；Regulation reaction temperature is 60～90 DEG C and can promote that pectin molecule moves, and is conducive to its dissolution；Selective retention molecular weight 5000～10000
The ultrafilter membrane of Da, utilizes pectin molecule amount to realize desalination with the significant difference of molecules of salt amount.
For achieving the above object, the present invention is realized by techniques below:
A kind of method extracting natural low methoxyl pectin from sunflower plate, the method step is as follows:
(1) washing: sunflower plate is pulverized the powder for passing through 60～80 mesh sieves, at normal temperatures, by the solid-liquid ratio of 1: 15～1: 30, will be to day
Certain herbaceous plants with big flowers dish powder is added to the water, and stirs 20～30min with 100～150 turns/min, filters with 200 mesh nylon gauzes afterwards, take filter cake；
(2) extract: the solid-liquid ratio (sunflower plate dry powder: water) according to 1: 20～1: 50, the sunflower plate wet feed after water washed be dispersed in water,
Be subsequently adding 0.4～1.0% (sodium citrate: water) sodium citrate as extractant, and with acid regulation system pH be 2～4, at 60～90 DEG C with
100～150 turns/min stirring extracts 1～4h, filters with 200 mesh nylon gauzes afterwards, takes filtrate；
(3) ultrafiltration desalination: with ultrafiltration, gained filtrate being carried out desalination, operation pressure is 5～20bar, and temperature is 10～40 DEG C, when system electrical conductivity
When being reduced to 500 below μ s/cm, stop ultrafiltration, reclaim trapped fluid, and temporarily retain filtered solution；
(4) ion exchange: by first adding anion exchange resin, the rear order adding cation exchange resin, add in ultrafiltration gained trapped fluid
Adding resin, be stirred at 20～30 DEG C, resin anion (R.A.) addition is 40～70g/L, mixing time 15～30min；Cationic resin addition
It is 5～20g/L, mixing time 15～30min；
(5) it is spray-dried: being spray-dried by the pectin solution after ion-exchange treatment, inlet temperature is 180～200 DEG C, and leaving air temp is
60～80 DEG C, flow velocity is 10～20mL/min, can obtain the powder pectin product that particle diameter is 5～10 microns；
(6) reverse osmosis: membrance separation gained filtered solution carries out reverse-osmosis treated, and operation pressure is 5～20bar, and temperature is 10～40 DEG C, works as filtration
When liquid electrical conductivity is higher than 500 μ s/cm, stops reverse osmosis, take trapped fluid；
(7) reclaim calcium citrate: under room temperature, in reverse osmosis trapped fluid, add solid calcium hydroxide or aqua calcis, until system pH is
Neutrality, obtains calcium citrate precipitation by filtering or being centrifuged, and obtains white calcium citrate powder at 60～80 DEG C after drying.
Especially, described extractant is sodium citrate, and acid used can be that citric acid, hydrochloric acid, sulphuric acid, nitric acid is therein a kind of or they mixed
Compound.
Especially, described ultrafilter membrane be molecular cut off be polysulfone membrane or the ceramic membrane of 5000～100000Da.
Especially, described anion exchange resin, it is specially by styrene and divinylbenzene crosslinking copolymerization, with sulfonic macroporous structure tree
Fat；Cation exchange resin, is specially by styrene and divinylbenzene crosslinking copolymerization, with the macroporous structure resin of quaternary ammonium group.
Beneficial effects of the present invention: using this method technique, in sunflower plate, natural low methoxyl pectin extraction ratio can reach 10～15% (by galacturonic acid
Acid meter, to raw material), ultrafiltration desalination can remove the salinity of more than 90%, and prepared low methoxyl pectin esterification degree is 25～30%, and amidation degree is 3～10%,
Galacturonic acid content 65～80% (to pectin), weight average molecular weight 200～300kDa.Sodium citrate is compared to ammonium oxalate, phosphate, ethylenediamine
The chelating agen such as tetraacethyl disodium, have greater security, add calcium hydroxide and can realize reclaiming calcium citrate after reverse osmosis.Compare traditional ethanol
The sedimentation method, this method technique is simpler, energy-saving and environmental protection.
Detailed description of the invention
In order to be more fully understood that the present invention, it is further elucidated with present disclosure below in conjunction with embodiment, but present disclosure is not limited solely to down
The embodiment in face.
Embodiment 1
(1) washing: 20g is crossed the sunflower plate powder of 60 mesh sieves, at normal temperatures, joins in 400mL deionized water, with 100 turns/min
Stirring 30min, filters with 200 mesh nylon gauzes afterwards, takes filter cake；
(2) extract: the sunflower plate wet feed after water washed is dispersed in 800mL 0.6% sodium citrate solution, and by sulphuric acid regulation system pH
It is 2.50, at 80 DEG C, extracts 2h with 100 turns/min stirring, filter with 200 mesh nylon gauzes afterwards, take filtrate；
(3) ultrafiltration desalination: with ultrafiltration, gained filtrate being carried out desalination, operation pressure is 12bar, and temperature is 25 DEG C, when system electrical conductivity reduces
During to 500 below μ s/cm, stop ultrafiltration, reclaim trapped fluid, and temporarily retain filtered solution；
(4) ion exchange: by first adding anion exchange resin, the rear order adding cation exchange resin, add in ultrafiltration gained trapped fluid
Adding resin, be stirred at 25 DEG C, resin anion (R.A.) addition is 50g/L, mixing time 30min；Cationic resin addition is 10g/L,
Mixing time 30min；
(5) it is spray-dried: being spray-dried by the pectin solution after ion-exchange treatment, inlet temperature is 180 DEG C, and leaving air temp is 65 DEG C,
Flow velocity is 15mL/min, can obtain powder pectin product, and yield is 11% (based on galacturonic acid, to raw material), and esterification degree is 21%, amide
Change degree 3%, weight average molecular weight 216kDa.
Embodiment 2
(1) washing: 80g is crossed the sunflower plate powder of 60～80 mesh sieves, at normal temperatures, joins in 1500mL deionized water, with 150 turns
/ min stirs 20min, filters with 200 mesh nylon gauzes afterwards, takes filter cake；
(2) extract: the sunflower plate wet feed after water washed is dispersed in 3500mL 0.8% sodium citrate solution, and by sulphuric acid regulation system pH
It is 3.00, at 90 DEG C, extracts 2.5h with 150 turns/min stirring, filter with 200 mesh nylon gauzes afterwards, take filtrate；
(3) ultrafiltration desalination: with ultrafiltration, gained filtrate being carried out desalination, operation pressure is 18bar, and temperature is 40 DEG C, when system electrical conductivity reduces
During to 500 below μ s/cm, stop ultrafiltration, reclaim trapped fluid, and temporarily retain filtered solution；
(4) ion exchange: by first adding anion exchange resin, the rear order adding cation exchange resin, add in ultrafiltration gained trapped fluid
Adding resin, be stirred at 30 DEG C, resin anion (R.A.) addition is 60g/L, mixing time 20min；Cationic resin addition is 15g/L,
Mixing time 20min；
(5) it is spray-dried: being spray-dried by the pectin solution after ion-exchange treatment, inlet temperature is 200 DEG C, and leaving air temp is 75 DEG C,
Flow velocity is 18mL/min, can obtain powder pectin product, and yield is 12% (in terms of galacturonic acid, to raw material), and esterification degree is 27%, amide
Change degree 5%, weight average molecular weight 247kDa.
Claims (4)
1. the method extracting natural low methoxyl pectin from sunflower plate, it is characterised in that comprise the following steps:
(1) washing: sunflower plate is pulverized the powder for passing through 60～80 mesh sieves, at normal temperatures, by the solid-liquid ratio of 1: 15～1: 30, by sunflower plate
Powder is added to the water, and stirs 20～30 minutes with 100～150 turns/min, filters with 200 mesh nylon gauzes afterwards, take filter cake；
(2) extract: the solid-liquid ratio (sunflower plate dry powder: water) according to 1: 20～1: 50, the sunflower plate wet feed after water washed is dispersed in water, so
Rear addition 0.4～1.0% (sodium citrate: water) sodium citrate are as extractant, and are 2～4 by acid regulation system pH, with 100～150 at 60～90 DEG C
Turn/min stirring extraction 1～4h, filter with 200 mesh nylon gauzes afterwards, take filtrate；
(3) ultrafiltration desalination: with ultrafiltration, gained filtrate being carried out desalination, operation pressure is 5～20bar, and temperature is 10～40 DEG C, when system electrical conductivity reduces
During to 500 below μ s/cm, stop ultrafiltration, reclaim trapped fluid, and temporarily retain filtered solution；
(4) ion exchange: by first adding anion exchange resin, the rear order adding cation exchange resin, in ultrafiltration gained trapped fluid, add tree
Fat is also stirred, and resin anion (R.A.) addition is 40～70g/L, mixing time 15～30min；Cationic resin addition is 5～20g/L, stirs
Mix the time 15～30min；
(5) it is spray-dried: being spray-dried by the pectin solution after ion-exchange treatment, inlet temperature is 180～200 DEG C, and leaving air temp is 60～80 DEG C,
Flow velocity is 10～20mL/min, can obtain the powder pectin product that particle diameter is 5～10 μm；
(6) reverse osmosis: membrance separation gained filtered solution carries out reverse-osmosis treated, and operation pressure is 5～20bar, and temperature is 10～40 DEG C, when filtered solution electricity
When conductance is higher than 500 μ s/cm, stops reverse osmosis, take trapped fluid；
(7) reclaim calcium citrate: under room temperature, in reverse osmosis trapped fluid, add solid calcium hydroxide or aqua calcis, until system pH is neutral,
Obtain calcium citrate precipitation by filtering or being centrifuged, after drying at 60～80 DEG C, obtain white calcium citrate powder.
A kind of method extracting natural low methoxyl pectin from sunflower plate, it is characterised in that the extractant described in step (2)
For sodium citrate, acid used can be that citric acid, hydrochloric acid, sulphuric acid, nitric acid is therein a kind of or their mixture.
A kind of method extracting natural low methoxyl pectin from sunflower plate, it is characterised in that the ultrafiltration institute described in step (3)
Ultrafilter membrane be molecular cut off be polysulfone membrane or the ceramic membrane of 5000～100000Da.
A kind of method extracting natural low methoxyl pectin from sunflower plate, it is characterised in that the anion described in step (4)
Exchanger resin, is specially by styrene and divinylbenzene crosslinking copolymerization, with sulfonic macroporous structure resin；Cation exchange resin, specifically
For by styrene and divinylbenzene crosslinking copolymerization, with the macroporous structure resin of quaternary ammonium group.
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| CN104151445B true CN104151445B (en) | 2016-08-24 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105884928B (en) * | 2016-04-26 | 2018-05-25 | 华中农业大学 | A kind of method that ammonium exchange process prepares low-ester pectin |
| CN105777936B (en) * | 2016-05-19 | 2018-06-22 | 江南大学 | A kind of low-ester pectin and preparation method thereof |
| CN106519068B (en) * | 2016-12-27 | 2019-06-11 | 晨光生物科技集团股份有限公司 | A kind of industrialized preparing process of sunflower plate low-ester pectin |
| CN107474157A (en) * | 2017-08-28 | 2017-12-15 | 广西钟山县富强雅瑶华香农业有限公司 | A kind of extracting method of sunflower pectin |
| CN107628944B (en) * | 2017-11-02 | 2023-10-24 | 厦门福美科技有限公司 | Method and system for extracting low-ester pectin and calcium citrate from passion fruit shells |
| CN109608562A (en) * | 2019-01-07 | 2019-04-12 | 中北大学 | A method of pectin being extracted from sunflower blueness disk using salt |
| CN109762076B (en) * | 2019-01-28 | 2020-04-17 | 江南大学 | Method for simultaneously extracting pectin and protein from sunflower discs |
| RU2706483C1 (en) * | 2019-03-22 | 2019-11-19 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Кубанский государственный аграрный университет имени И.Т. Трубилина" | Method for production of pectin extract from sunflower clusters |
| TWI717827B (en) * | 2019-09-09 | 2021-02-01 | 侯士國 | Low methoxyl pectin from jelly-fig (ficus pumila l. var. awkeotsang (makino) corner) and method for producing the same |
| CN110833194B (en) * | 2019-10-28 | 2023-01-24 | 中北大学 | Controlled-release sunflower disc low-ester pectin iron composite iron supplement and preparation method thereof |
| CN111349183B (en) * | 2020-04-22 | 2022-04-01 | 黑龙江八一农垦大学 | Pectin and its extraction method and preparation method |
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| CN101037484A (en) * | 2007-04-02 | 2007-09-19 | 范兆科 | Method for separating low methoxyl pectin from sunflower plate by using membrane technology |
| CN102304192A (en) * | 2011-04-09 | 2012-01-04 | 吕维学 | Method for extracting low-ester pectin from sunflower heads and stems and ultrafiltration device |
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| JPS6465101A (en) * | 1987-09-05 | 1989-03-10 | Takeshi Ishii | Water hyacinth pectin |
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2014
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| WO1997049298A1 (en) * | 1996-06-24 | 1997-12-31 | Societe Des Produits Nestle S.A. | Pectinaceous gelling agent |
| CN101037484A (en) * | 2007-04-02 | 2007-09-19 | 范兆科 | Method for separating low methoxyl pectin from sunflower plate by using membrane technology |
| CN102304192A (en) * | 2011-04-09 | 2012-01-04 | 吕维学 | Method for extracting low-ester pectin from sunflower heads and stems and ultrafiltration device |
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