CN104151445A - Method for extracting natural low-ester pectin from sunflower heads - Google Patents
Method for extracting natural low-ester pectin from sunflower heads Download PDFInfo
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Abstract
The invention relates to a method for extracting natural low-ester pectin from sunflower heads. The method comprises the following steps: washing; extracting; carrying out ultrafiltration desalination; carrying out ion exchange to remove residual salt; carrying out spray drying; carrying out reverse osmosis; and recovering calcium citrate, wherein a chelating agent used for extraction is sodium citrate, the concentration is 0.4%-1.0% (sodium citrate: water), the extraction solid-to-liquid ratio is 1:20-1:50 (sunflower head dry powder: water), the pH is regulated to 2-4, then a great part of salt is removed by using an ultrafiltration membrane with the interception molecular weight of 5000-10000 Da, and the residual salt is removed by adopting the ion exchange. The method disclosed by the invention can achieve the pectin extraction rate by 10%-15% (in terms of galacturonic acid on raw materials) and is capable of removing the salt by more than 90% through the ultrafiltration desalination; and as for the prepared low-ester pectin, the esterification degree is 25%-30%, the amidation degree is 3%-10%, the content of the galacturonic acid is 65%-80% (on the pectin), and the weight-average molecular weight is 200-300 kDa. According to the method, the sodium citrate as the chelating agent has very high safety and can realize calcium citrate recovery through the addition of calcium hydroxide after reverse osmosis.
Description
Technical field
The invention belongs to food colloid field, particularly a kind of novel chelating agents extracts the preparation method in conjunction with the natural low-ester pectin of ultrafiltration purification.
Background technology
Pectin is a kind of complex construction polysaccharide being extensively present in terrestrial plant cell walls.In the food-processings such as bakery, yogurt drink, fruit juice, pectin is as hydrophilic colloid, has the effects such as gelling, stable and thickening.Meanwhile, pectin is also natural water-soluble dietary fibre, has the human body of adjusting intestinal microenvironment, reduces the beneficial functionals such as blood fat.
Pectin can be divided into high ester pectin (gamma value >50%) and low-ester pectin (gamma value <50%).Business pectin mostly is high ester pectin at present, and its raw material is mainly tangerine section fruit skin slag, apple peel and beet skin slag etc.Low-ester pectin as stablizer, gelifying agent and thickening material can unique application in low sugar, low-calorie functionality food, as the production of the jam of low sugar, jelly, soft sweets, frozen confection, ice-creams, Yoghourt pulp bed material, baked goods glazing etc.Approximately 5000 tons/year of the current global low-ester pectin market requirements, and with 10～20% speed increase.Pectin in sunflower plate is natural low-ester pectin, and China's sunflower planting area reaches 960000m
2, contain abundant natural low-ester pectin resource.
After current industrial pectin extraction method is mainly acid system and extracts, then by ethanol precipitation, utilize acid hydrolysis cell walls to discharge pectin, the characteristic of utilizing afterwards pectin to be insoluble to alcohol realizes separating of pectin and other materials.Wherein, acid system often adds the sequestrant assisted extraction such as disodium ethylene diamine tetraacetate, phosphoric acid salt, ammonium oxalate in extracting, but can improve pectin aftertreatment cost and cause security risk; Ethanol precipitation process need expend a large amount of ethanol, causes to reclaim that energy consumption is large, environment protection treating high in cost of production problem.Therefore, can consider to adopt the Physical Separation Technology of the safely cleanings such as membrane sepn to carry out separation and purification to pectin.
Summary of the invention
The object of this invention is to provide a kind of industrialization, safe and simple natural low-ester pectin technology of preparing of being easy to, adopt Trisodium Citrate to extract in conjunction with the method for ultrafiltration purification and extract pectin, in obtaining high extraction and high purity product, improve Product Safety, reduce production costs, eliminate environmental issue.
Principle of the present invention is: natural pectin and Ca
2+form chelation structure, be unfavorable for pectin extraction.Trisodium Citrate as sequestrant can capture with pectin in the Ca of complexing
2+, promote that pectin is soluble in water; Regulating reaction pH is 2～4 Mierocrystalline cellulose and hemicelluloses in can partial hydrolysis cell walls, favourable pectin stripping; Regulate temperature of reaction to be 60～90 DEG C and can promote pectin molecule motion, be conducive to its stripping; The ultra-filtration membrane of selective retention molecular weight 5000～10000Da, utilizes the significant difference of pectin molecule amount and molecules of salt amount to realize desalination.
For achieving the above object, the present invention realizes by following technology:
From sunflower plate, extract a method for natural low-ester pectin, the method step is as follows:
(1) washing: sunflower plate is pulverized as can pass through the powder of 60～80 mesh sieves, at normal temperatures, by the solid-liquid ratio of 1: 15～1: 30, sunflower plate powder is added to the water, stir 20～30min with 100～150 turn/min, filter with 200 order nylon gauzes afterwards, get filter cake;
(2) extract: according to the solid-liquid ratio of 1: 20～1: 50 (sunflower plate dry powder: water), washing sunflower plate wet feed is later dispersed in water, then add 0.4～1.0% (Trisodium Citrate: water) Trisodium Citrate as extraction agent, and with sour regulation system pH be 2～4, at 60～90 DEG C, stir and extract 1～4h with 100～150 turn/min, filter with 200 order nylon gauzes afterwards, get filtrate;
(3) ultrafiltration desalination: with ultrafiltration, gained filtrate is carried out to desalination, working pressure is 5～20bar, and temperature is 10～40 DEG C, below system specific conductivity is reduced to 500 μ s/cm time, stops ultrafiltration, reclaims trapped fluid, and temporarily retains filtered solution;
(4) ion-exchange: by first adding anionite-exchange resin, the order of rear interpolation Zeo-karb is added resin in ultrafiltration gained trapped fluid, stirs at 20～30 DEG C, resin anion(R.A) addition is 40～70g/L, churning time 15～30min; Resin cation (R.C.) addition is 5～20g/L, churning time 15～30min;
(5) spraying is dry: the pectin solution after ion exchange treatment spray and is dried, and inlet temperature is 180～200 DEG C, and air outlet temperature is 60～80 DEG C, and flow velocity is 10～20mL/min, can obtain particle diameter and be the powder pectin product of 5～10 microns;
(6) reverse osmosis: membrane sepn gained filtered solution is carried out to reverse-osmosis treated, and working pressure is 5～20bar, and temperature is 10～40 DEG C, when filtered solution specific conductivity is during higher than 500 μ s/cm, stops reverse osmosis, gets trapped fluid;
(7) reclaim citrate of lime: under normal temperature, in reverse osmosis trapped fluid, add solid hydrogen calcium oxide or aqua calcis, until system pH is neutral, by filtering or the centrifugal citrate of lime precipitation that obtains, after drying, obtain white citrate of lime powder at 60～80 DEG C.
Especially, described extraction agent is Trisodium Citrate, and acid used can be wherein a kind of such as citric acid, hydrochloric acid, sulfuric acid, nitric acid or their mixture.
Especially, described ultra-filtration membrane is that molecular weight cut-off is polysulfone membrane or the ceramic membrane of 5000～100000Da.
Especially, described anionite-exchange resin, is specially by vinylbenzene and divinylbenzene crosslinking copolymerization, with sulfonic macroporous structure resin; Zeo-karb, is specially by vinylbenzene and divinylbenzene crosslinking copolymerization, with the macroporous structure resin of quaternary ammonium group.
Beneficial effect of the present invention: use present method technique, in sunflower plate, natural low-ester pectin extraction yield can reach 10～15% (by galacturonic acid, to raw material), ultrafiltration desalination can remove more than 90% salinity, the low-ester pectin gamma value making is 25～30%, amidation degree is 3～10%, galacturonic acid content 65～80% (to pectin), weight-average molecular weight 200～300kDa.Trisodium Citrate, than sequestrants such as ammonium oxalate, phosphoric acid salt, disodium ethylene diamine tetraacetate, has greater security, adds calcium hydroxide can realize recovery citrate of lime after reverse osmosis.Compare traditional ethanol precipitation, present method technique is simpler, energy-saving and environmental protection.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1
(1) washing: 20g is crossed to the sunflower plate powder of 60 mesh sieves, at normal temperatures, join in 400mL deionized water, stir 30min with 100 turn/min, filter with 200 order nylon gauzes afterwards, get filter cake;
(2) extract: washing sunflower plate wet feed is later dispersed in 800mL0.6% sodium citrate solution, and with sulfuric acid regulation system pH be 2.50, at 80 DEG C, stir and extract 2h with 100 turn/min, with 200 order nylon gauzes filtrations, get filtrate afterwards;
(3) ultrafiltration desalination: with ultrafiltration, gained filtrate is carried out to desalination, working pressure is 12bar, and temperature is 25 DEG C, below system specific conductivity is reduced to 500 μ s/cm time, stops ultrafiltration, reclaims trapped fluid, and temporarily retains filtered solution;
(4) ion-exchange: by first adding anionite-exchange resin, the order of rear interpolation Zeo-karb is added resin in ultrafiltration gained trapped fluid, stirs at 25 DEG C, and resin anion(R.A) addition is 50g/L, churning time 30min; Resin cation (R.C.) addition is 10g/L, churning time 30min;
(5) spraying is dry: the pectin solution after ion exchange treatment is sprayed dry, inlet temperature is 180 DEG C, air outlet temperature is 65 DEG C, flow velocity is 15mL/min, can obtain powder pectin product, and yield is 11% (by galacturonic acid, to raw material), gamma value is 21%, amidation degree 3%, weight-average molecular weight 216kDa.
Embodiment 2
(1) washing: 80g is crossed to the sunflower plate powder of 60～80 mesh sieves, at normal temperatures, join in 1500mL deionized water, stir 20min with 150 turn/min, filter with 200 order nylon gauzes afterwards, get filter cake;
(2) extract: washing sunflower plate wet feed is later dispersed in 3500mL0.8% sodium citrate solution, and with sulfuric acid regulation system pH be 3.00, at 90 DEG C, stir and extract 2.5h with 150 turn/min, filter with 200 order nylon gauzes afterwards, get filtrate;
(3) ultrafiltration desalination: with ultrafiltration, gained filtrate is carried out to desalination, working pressure is 18bar, and temperature is 40 DEG C, below system specific conductivity is reduced to 500 μ s/cm time, stops ultrafiltration, reclaims trapped fluid, and temporarily retains filtered solution;
(4) ion-exchange: by first adding anionite-exchange resin, the order of rear interpolation Zeo-karb is added resin in ultrafiltration gained trapped fluid, stirs at 30 DEG C, and resin anion(R.A) addition is 60g/L, churning time 20min; Resin cation (R.C.) addition is 15g/L, churning time 20min;
(5) spraying is dry: the pectin solution after ion exchange treatment is sprayed dry, inlet temperature is 200 DEG C, air outlet temperature is 75 DEG C, flow velocity is 18mL/min, can obtain powder pectin product, and yield is 12% (in galacturonic acid, to raw material), gamma value is 27%, amidation degree 5%, weight-average molecular weight 247kDa.
Claims (4)
1. a method of extracting natural low-ester pectin from sunflower plate, is characterized in that comprising the following steps:
(1) washing: sunflower plate is pulverized as can pass through the powder of 60～80 mesh sieves, at normal temperatures, by the solid-liquid ratio of 1: 15～1: 30, sunflower plate powder is added to the water, stir 20～30 minutes with 100～150 turn/min, filter with 200 order nylon gauzes afterwards, get filter cake;
(2) extract: according to the solid-liquid ratio of 1: 20～1: 50 (sunflower plate dry powder: water), washing sunflower plate wet feed is later dispersed in water, then add 0.4～1.0% (Trisodium Citrate: water) Trisodium Citrate as extraction agent, and with sour regulation system pH be 2～4, at 60～90 DEG C, stir and extract 1～4h with 100～150 turn/min, filter with 200 order nylon gauzes afterwards, get filtrate;
(3) ultrafiltration desalination: with ultrafiltration, gained filtrate is carried out to desalination, working pressure is 5～20bar, and temperature is 10～40 DEG C, below system specific conductivity is reduced to 500 μ s/cm time, stops ultrafiltration, reclaims trapped fluid, and temporarily retains filtered solution;
(4) ion-exchange: by first adding anionite-exchange resin, the order of rear interpolation Zeo-karb is added resin and stirs in ultrafiltration gained trapped fluid, and resin anion(R.A) addition is 40～70g/L, churning time 15～30min; Resin cation (R.C.) addition is 40～70g/L, 5～20g/L, churning time 15～30min;
(5) spraying is dry: the pectin solution after ion exchange treatment is sprayed dry, inlet temperature is 180～200 DEG C, and air outlet temperature is 60～80 DEG C, and flow velocity is 10～20mL/min, and can obtain particle diameter is the powder pectin product of 5～10 μ m;
(6) reverse osmosis: membrane sepn gained filtered solution is carried out to reverse-osmosis treated, and working pressure is 5～20bar, and temperature is 10～40 DEG C, when filtered solution specific conductivity is during higher than 500 μ s/cm, stops reverse osmosis, gets trapped fluid;
(7) reclaim citrate of lime: under normal temperature, in reverse osmosis trapped fluid, add solid hydrogen calcium oxide or aqua calcis, until system pH is neutral, by filtering or the centrifugal citrate of lime precipitation that obtains, after drying, obtain white citrate of lime powder at 60～80 DEG C.
2. a kind of method of extracting natural low-ester pectin from sunflower plate as claimed in claim 1, it is characterized in that the described extraction agent of step (2) is Trisodium Citrate, acid used can be wherein a kind of such as citric acid, hydrochloric acid, sulfuric acid, nitric acid or their mixture.
3. a kind of method of extracting natural low-ester pectin from sunflower plate as claimed in claim 1, is characterized in that the described ultra-filtration membrane of step (3) is that molecular weight cut-off is polysulfone membrane or the ceramic membrane of 5000～100000Da.
4. a kind of method of extracting natural low-ester pectin from sunflower plate as claimed in claim 1, it is characterized in that the anionite-exchange resin that step (4) is described, be specially by vinylbenzene and divinylbenzene crosslinking copolymerization, with sulfonic macroporous structure resin; Zeo-karb, is specially by vinylbenzene and divinylbenzene crosslinking copolymerization, with the macroporous structure resin of quaternary ammonium group.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777936A (en) * | 2016-05-19 | 2016-07-20 | 江南大学 | Low-ester pectin and preparation method thereof |
| CN105884928A (en) * | 2016-04-26 | 2016-08-24 | 华中农业大学 | Method using ammonium exchange method to prepare low-methoxyl pectin |
| CN106519068A (en) * | 2016-12-27 | 2017-03-22 | 晨光生物科技集团股份有限公司 | Industrial production method of sunflower head 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 |
| CN107628944A (en) * | 2017-11-02 | 2018-01-26 | 厦门福美科技有限公司 | The method and system of low-ester pectin and calcium citrate is extracted from passion fruit shell |
| CN109608562A (en) * | 2019-01-07 | 2019-04-12 | 中北大学 | A method of pectin being extracted from sunflower blueness disk using salt |
| CN109762076A (en) * | 2019-01-28 | 2019-05-17 | 江南大学 | A method of extracting pectin and protein simultaneously from sunflower plate |
| 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 |
| CN110833194A (en) * | 2019-10-28 | 2020-02-25 | 中北大学 | Controlled-release sunflower disc low-ester pectin iron composite iron supplement and preparation method thereof |
| CN111303312A (en) * | 2019-09-09 | 2020-06-19 | 侯士国 | Low-methoxy pectin of Ficus awkeotsang Makino and preparation method thereof |
| CN111349183A (en) * | 2020-04-22 | 2020-06-30 | 黑龙江八一农垦大学 | Pectin and its extraction method and preparation method |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105884928A (en) * | 2016-04-26 | 2016-08-24 | 华中农业大学 | Method using ammonium exchange method to prepare low-methoxyl pectin |
| 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 |
| CN105777936A (en) * | 2016-05-19 | 2016-07-20 | 江南大学 | Low-ester pectin and preparation method thereof |
| CN106519068A (en) * | 2016-12-27 | 2017-03-22 | 晨光生物科技集团股份有限公司 | Industrial production method of sunflower head 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 |
| CN107628944A (en) * | 2017-11-02 | 2018-01-26 | 厦门福美科技有限公司 | The method and system of low-ester pectin and calcium citrate is extracted from passion fruit shell |
| CN109608562A (en) * | 2019-01-07 | 2019-04-12 | 中北大学 | A method of pectin being extracted from sunflower blueness disk using salt |
| CN109762076A (en) * | 2019-01-28 | 2019-05-17 | 江南大学 | A method of extracting pectin and protein simultaneously from sunflower plate |
| 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 |
| CN111303312A (en) * | 2019-09-09 | 2020-06-19 | 侯士国 | Low-methoxy pectin of Ficus awkeotsang Makino and preparation method thereof |
| CN111303312B (en) * | 2019-09-09 | 2022-05-31 | 侯士国 | Low-methoxy pectin of Ficus awkeotsang Makino and preparation method thereof |
| CN110833194A (en) * | 2019-10-28 | 2020-02-25 | 中北大学 | Controlled-release sunflower disc low-ester pectin iron composite iron supplement and preparation method thereof |
| 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 |
| CN111349183A (en) * | 2020-04-22 | 2020-06-30 | 黑龙江八一农垦大学 | Pectin and its extraction method and preparation method |
| 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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