CN102643366A - Production method of high-ester pectin by intermittent acid extraction and ethanol precipiration - Google Patents
Production method of high-ester pectin by intermittent acid extraction and ethanol precipiration Download PDFInfo
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Abstract
The invention discloses a production method of high-ester pectin by intermittent acid extraction and ethanol precipiration, which comprises the following steps: soaking dried orange peel in 45 DEG C warm water for 30 minutes until the dried orange peel absorbs sufficient water and is softened to remove soluble impurities; draining the orange peel, putting the orange peel in boiling water to inactivate enzymes, rinsing the orange peel subjected to enzyme inactivation in running water to no color, and pulverizing with a pulverizer; extracting the pulverized orange peel particles and water in a mass ratio of 1:(5-20) at 50-90 DEG C for 30-90 minutes while controlling the pH value within 1.0-3.0, and filtering; carrying out vacuum rotary evaporation on the filtrate; adding anhydrous ethanol into the concentrated solution, precipitating and carrying out vacuum filtration to obtain a filter cake; and drying the filter cake at 40 DEG C to obtain the high-ester pectin. The high-ester pectin obtained by the production method disclosed by the invention has better gelation properties than the commercially available high-ester pectin produced in China. The high-ester pectin appears as a pseudoplastic fluid when the solution concentration is high.
Description
Technical field
The present invention relates to a kind of working method of high ester pectin of intermittent type acid extraction ethanol sedimentation.
Background technology
Pectin is a kind of natural additive for foodstuff of totally nontoxic, is to receive FAO/WHO foodstuff additive joint committee to recommend the generally regarded as safe foodstuff additive of GMP (good manufacturing practice).Owing to having remarkable gelation and emulsifying stability, pectin make it become a kind of important additive in the foodstuffs industry.Up-to-date research shows, pectin has effects such as diarrhea, anticancer, treatment mellitus as soluble dietary fibre, and its range of application is enlarging.In addition, pectin all has significant effect in various reaction mechanisms and metabolic pathway, and this also makes pectin become some medicines and healthcare products and the central indispensable auxiliary material of makeup.
In China since import pectin price far above homemade pectin, therefore homemade pectin has become the expectation of numerous domestic enterprise, develops the pectin resource of China's abundant energetically, produces high-quality pectin, satisfies the domestic and international market demand and has seemed very urgent.
Yet China's pectin production status is at present: manufacturing enterprise is few in number, and industrial scale is little, and production technology process is backward relatively, and quality products is few.According to the domestic and international process for processing trend of pectin at present, research and develop out rational production technique as early as possible, make full use of the pectin resource of China's abundant.The acid extraction salting-out process yields poorly in the method for extraction high ester pectin at present, be merely about 7%, and the little difficult separation of aluminium salt deposit seeds, high price molysite color is darker, needs do decolouring processing.
Summary of the invention
The object of the invention provides a kind of working method of high ester pectin of intermittent type acid extraction ethanol sedimentation in order to solve above-mentioned technical problem.It is simple that the working method of the high ester pectin of this intermittent type acid extraction ethanol sedimentation has technology, and gained high ester pectin purity is high, and color and luster is good, and productive rate is high, and to do matter, productive rate is up to 20%～30%.
Technical scheme of the present invention
A kind of working method of high ester pectin of intermittent type acid extraction ethanol sedimentation comprises the following steps:
(1), the pre-treatment of tangerine peel
Take by weighing dried tangerine peel 20g; Be soaked in about 30min in 45 ℃ of warm water; It is softening that it is fully absorbed water, and removes soluble impurity, drains tangerine peel and put into boiling water and boil the 10min enzyme that goes out; The tangerine peel that goes out behind the enzyme places the flowing water rinsing to colourless, uses kibbler to be crushed to the tangerine peel particle of particle diameter as 1-5mm then;
(2), acid hydrolysis
Get step (1) with the tangerine peel particle after pulverizing; By itself and the calculating of the mass ratio of water; Be the tangerine peel particle: water be 1:5-20 mix the back uses concentration as the hydrochloric acid soln of 5mol/L regulate the pH value as 1.0-3.0, controlled temperature as 50-90 ℃ of extraction 30-90min after-filtration, filtrating is carried out rotary evaporation in vacuo, obtain liquid concentrator after; The absolute ethyl alcohol that adds 3-5 times of volume again, suction filtration behind the deposition 1h;
(3), drying
The filter cake that obtains behind step (2) suction filtration is carried out drying under 40 ℃ of temperature, finally obtain high ester pectin.
Beneficial effect of the present invention
The working method of the high ester pectin of a kind of intermittent type acid extraction ethanol sedimentation of the present invention, not only production technique is simple, and gained high ester pectin purity is high, and color and luster is good, and productive rate is calculated as 20%-30% to do matter.
The high ester pectin of the working method gained of the high ester pectin of a kind of intermittent type acid extraction ethanol sedimentation of the present invention; At gelation condition is that sugared content is 55%; Citric acid concentration is 0.5mol/L, and concentration of pectin is 1.00% o'clock, and its each side gellifying property all is superior to the performance of commercially available homemade high ester pectin.
In addition, from rheological property, when the concentration of the high ester pectin solution of working method gained of the present invention was high more, it is big more that viscosity is influenced by shearing force.Under the same concentrations, the viscosity of the high ester pectin of working method gained of the present invention is less than commercially available homemade high ester pectin with the variation of shearing force.In the uniform temp variation range, the high ester pectin temperature influence of working method gained of the present invention is less than commercially available homemade high ester pectin.
Description of drawings
Under Fig. 1, the same concentrations, the comparison of the rheological property of the high ester pectin of commercially available homemade, commercially available import high ester pectin and embodiment 5 gained;
The viscosity of the high ester pectin solution of embodiment 5 gained receives the graphic representation of influence of temperature change under Fig. 2, the differing temps;
In Fig. 3, the uniform temp variation range, the viscosity of commercially available homemade high ester pectin receives the graphic representation of influence of temperature change;
In Fig. 4, the uniform temp variation range, the viscosity of commercially available import high ester pectin receives the graphic representation of influence of temperature change.
Embodiment
Below through embodiment and combine accompanying drawing that the present invention is further set forth, but do not limit the present invention.
For realizing the working method of a kind of intermittent type acid extraction high ester pectin of the present invention, the model of the instrument that various embodiments of the present invention are used and the information of manufacturer are following:
Medical Equipment Plant of electric-heated thermostatic water bath HHS Shanghai Boxun Industrial Co., Ltd.
The accurate pH meter of pHS-36 type Shanghai Precision & Scientific Instrument Co., Ltd. Leici Instrument Factory
The grand experimental installation of Nereid ltd on the electric heating constant temperature air dry oven PHG-9146A type
Constant temperature bath W201S Shensheng Science & Tech. Co., Ltd., Shanghai
Recirculated water vacuum pump SHB-3 Shensheng Science & Tech. Co., Ltd., Shanghai
Rotatory evaporator R series Shensheng Science & Tech. Co., Ltd., Shanghai
Single phase ac induction motor Shensheng Science & Tech. Co., Ltd., Shanghai
Separating centrifuge Shanghai City laboratory apparatus head factory
Kibbler Shanghai Rui Xin electrical apparatus factory
Electronic scale Shanghai Precision Scientific Apparatus Co., Ltd
Rheometer AG-R2 U.S. TA company
Matter structure appearance TA-XT plus Britain Stable Micro System company.
The used reagent of the present invention is homemade analytical pure, all available from Chemical Reagent Co., Ltd., Sinopharm Group; Commercially available homemade high ester pectin is available from Quzhou, Zhejiang pectin factory, and commercially available import high ester pectin is available from U.S. cpkelco company.
High ester pectin yield calculation formula:
Used dried tangerine peel is that the tangerine peel of collecting is carried out forced air drying in air dry oven in the embodiment of the invention, and drying temperature is 45 ℃, treat the tangerine peel complete drying after, put into moisture eliminator after the pack and deposit.
A kind of working method of high ester pectin of intermittent type acid extraction ethanol sedimentation comprises the following steps:
(1), the pre-treatment of tangerine peel
Take by weighing 5 parts of dried tangerine peels respectively; Every part of 20g is soaked in about 30min in 45 ℃ of warm water respectively, and it is softening that it is fully absorbed water; Remove soluble impurity; Drain tangerine peel and put into boiling water and boil the 10min enzyme that goes out, the tangerine peel behind the enzyme that goes out places the flowing water rinsing to colourless, uses kibbler to be crushed to the tangerine peel particle of particle diameter as 1-5mm then respectively;
(2), acid hydrolysis
Get step (1) respectively with the tangerine peel particle after pulverizing; By itself and the calculating of the mass ratio of water; Be the tangerine peel particle: water be 1:20 mix the back uses concentration as the hydrochloric acid soln of 5mol/L adjusting pH value be 1.5, controlled temperature is 80 ℃ of extraction times to be respectively 30min, 45min, 60min, 75min and 90min after-filtration, will filtrate and carry out rotary evaporation in vacuo respectively, obtain liquid concentrator after; The absolute ethyl alcohol that adds 3-5 times of volume more respectively, suction filtration behind the deposition 1h;
(3), drying
Respectively the filter cake that obtains behind step (2) suction filtration is carried out drying under 40 ℃ of temperature, finally obtain 5 kinds and be respectively 1.25g, 1.97g, 2.86g, the 3.19g of 30min, 45min, 60min, 75min and 90min, the high ester pectin of 3.23g corresponding to extraction time.
The above-mentioned high ester pectin yield that obtains under corresponding 5 kinds of different extraction times is 6.25%, 9.85%, 14.28%, 15.95%, 16.13%.This shows that extraction time increases to by 30min in the process of 90min, the high ester pectin yield constantly increases.Extraction time is too short, and the high ester pectin matter in the tangerine peel fails to be dissolved out fully, and extraction yield is lower; But extraction time is long, though output still increases to some extent, a small amount of low glycan molecule begins to take place browning reaction in the pericarp; Cause the extracting solution color to be isabelline; The high ester pectin quality is exerted an influence, so that extraction time should be controlled is suitable, the selective extraction time is preferable in the 75min left and right sides.
Embodiment 2
A kind of working method of high ester pectin of intermittent type acid extraction ethanol sedimentation comprises the following steps:
(1), the pre-treatment of tangerine peel
Take by weighing 5 parts of dried tangerine peels respectively; Every part of 20g is soaked in about 30min in 45 ℃ of warm water respectively, and it is softening that it is fully absorbed water; Remove soluble impurity; Drain tangerine peel and put into boiling water and boil the 10min enzyme that goes out, the tangerine peel behind the enzyme that goes out places the flowing water rinsing to colourless, uses kibbler to be crushed to the tangerine peel particle of particle diameter as 1-5mm then respectively;
(2), acid hydrolysis
The particle diameter of getting step (1) gained respectively is the tangerine peel particle of 1-5mm; By itself and the calculating of the mass ratio of water; Be the tangerine peel particle: water is that 1:20 mixes the back respectively and uses concentration to regulate as the hydrochloric acid soln of 5mol/L that the pH value is 1.5, controlled temperature is respectively 50 ℃, 60 ℃, 70 ℃, 80 ℃ and 90 ℃ of extraction 60min after-filtration, will filtrate and carry out rotary evaporation in vacuo respectively, obtain liquid concentrator after; The absolute ethyl alcohol that adds 3-5 times of volume more respectively, suction filtration behind the deposition 1h;
(3), drying
Respectively the filter cake that obtains behind step (2) suction filtration is carried out drying under 40 ℃ of temperature, finally obtain 5 kinds corresponding to the high ester pectin that extracts 2.03g that temperature is respectively 50 ℃, 60 ℃, 70 ℃, 80 ℃ and 90 ℃, 2.57g, 2.64g, 2.93g, 2.97g.
5 kinds of yield corresponding to the high ester pectin under the different extraction temperature of above-mentioned gained are respectively 10.15%, 12.85%, 13.18%, 14.65%, 14.83%.This shows the rising along with temperature, help the aquation stripping of high ester pectin, the high ester pectin yield constantly increases; But be not linear; And when temperature is too high, may cause the destruction of high ester pectin self structure, the macromolecule polysaccharide compound is degraded to some extent.When the extraction temperature was low, product production was low; When temperature was higher, product colour was deepened, and quality is affected, so that temperature generally is controlled at 80 ℃ of left and right sides is preferable.
A kind of working method of high ester pectin of intermittent type acid extraction ethanol sedimentation comprises the following steps:
(1), the pre-treatment of tangerine peel
Take by weighing 5 parts of dried tangerine peels respectively; Every part of 20g is soaked in about 30min in 45 ℃ of warm water respectively, and it is softening that it is fully absorbed water; Remove soluble impurity; Drain tangerine peel and put into boiling water and boil the 10min enzyme that goes out, the tangerine peel behind the enzyme that goes out places the flowing water rinsing to colourless, uses kibbler to be crushed to the tangerine peel particle of particle diameter as 1-5mm then respectively;
(2), acid hydrolysis
The particle diameter of getting step (1) gained respectively is 5 parts of tangerine peel particles of 1-5mm; Successively by itself and the calculating of the mass ratio of water; Be the tangerine peel particle: water is respectively and uses concentration to regulate as the hydrochloric acid soln of 5mol/L that pH value is 1.5, controlled temperature is 80 ℃ of extraction 60min after-filtration after 1:5,1:10,1:15,1:20 and 1:25 mix respectively, will filtrate and carry out rotary evaporation in vacuo respectively, obtain liquid concentrator after; The absolute ethyl alcohol that adds 3-5 times of volume more respectively, suction filtration behind the deposition 1h;
(3), drying
Respectively the filter cake that obtains behind step (2) suction filtration is carried out drying under 40 ℃ of temperature, finally obtaining 5 kinds of mass ratioes corresponding to tangerine peel particle and water is the tangerine peel particle: water is respectively 0.95g, 1.57g, 2.46g, the 2.82g of gained under the situation of 1:5,1:10,1:15,1:20 and 1:25, the high ester pectin of 2.87g.
Above-mentioned gained be that 5 kinds of mass ratioes corresponding to tangerine peel particle and water are the tangerine peel particle: the yield that water is respectively the high ester pectin under the situation of 1:5,1:10,1:15,1:20 and 1:25 is respectively 4.75%, 7.85%, 12.28%, 14.10%, 14.33%.This shows the increase along with the ratio of mixture of tangerine peel particle and water, it is big that the high ester pectin yield becomes gradually.When the ratio of mixture of tangerine peel particle and water was 1:5-10, the high ester pectin yield was very low, possibly be because the ratio of mixture of tangerine peel particle and water is too little; Be difficult to guarantee that the high ester pectin in the tangerine peel transfers in the liquid phase fully; And in filtration procedure, the material viscosity is big, has caused filtration difficulty.And the ratio of mixture of tangerine peel particle and water is when being 1:25, and the high ester pectin yield is in maximum, but for follow-up concentrating and precipitating process, concentration time is longer, and precipitation agent ethanol consumption is bigger, and sedimentation effect is undesirable.Thereby to select the preferable tangerine peel particle and the ratio of mixture of water, both guaranteed that all high ester pectins all were transferred to liquid phase, the energy consumption when improving the speed when filtering simultaneously and reducing evaporation concentration.So it is preferable that the ratio of mixture of tangerine peel particle and water generally is controlled at the 1:20 left and right sides.
A kind of working method of high ester pectin of intermittent type acid extraction ethanol sedimentation comprises the following steps:
(1), the pre-treatment of tangerine peel
Take by weighing 5 parts of dried tangerine peels respectively; Every part of 20g is soaked in about 30min in 45 ℃ of warm water respectively, and it is softening that it is fully absorbed water; Remove soluble impurity; Drain tangerine peel and put into boiling water and boil the 10min enzyme that goes out, the tangerine peel behind the enzyme that goes out places the flowing water rinsing to colourless, uses kibbler to be crushed to the tangerine peel particle of particle diameter as 1-5mm then respectively;
(2), acid hydrolysis
The particle diameter of getting step (1) gained respectively is 5 parts of tangerine peel particles of 1-5mm; Successively by itself and the calculating of the mass ratio of water; Be the tangerine peel particle: water is to use concentration to regulate as the hydrochloric acid soln of 5mol/L that pH value is 1.5, controlled temperature is 80 ℃ of extraction 60min after-filtration after 1:20 mixes respectively, will filtrate and carry out rotary evaporation in vacuo respectively, obtain liquid concentrator after; The absolute ethyl alcohol that adds 3-5 times of volume more respectively, suction filtration behind the deposition 1h;
(3), drying
The filter cake that obtains behind step (2) suction filtration is carried out drying respectively under 40 ℃ of the temperature, finally obtain 5 kinds corresponding to the high ester pectin that extracts 3.47g that the pH value is respectively gained under 1.0,1.5,2.0,2.5 and 3.0 the situation, 3.39g, 2.56g, 1.27g, 0.75g.
5 kinds of above-mentioned gained are respectively 17.33%, 16.95%, 12.82%, 6.35%, 3.73% corresponding to extracting the yield that the pH value is respectively the high ester pectin of gained under 1.0,1.5,2.0,2.5 and 3.0 the situation.This shows that the pH value is big more, the high ester pectin yield is more little.In experiment, when the pH value is 1.0 left and right sides, be dark-coloured, behind the adding ethanol sedimentation through the high ester pectin solution colour after the acidolysis; The bulk deposition occurs, after drying, obtain the coke black material; Peculiar smell is arranged, with finished product multiple water-soluble after, about 70% fails dissolving; So judgement pH value is that the product under 1.0 is not all to be high ester pectin, under the possible strong acid, degraded has also taken place in other material in the pericarp.When the pH value was 1.5 left and right sides, the high ester pectin extraction yield was higher.
A kind of working method of high ester pectin of intermittent type acid extraction ethanol sedimentation comprises the following steps:
(1), the pre-treatment of tangerine peel
Take by weighing dried tangerine peel 20g; Be soaked in about 30min in 45 ℃ of warm water; It is softening that it is fully absorbed water, and removes soluble impurity, drains tangerine peel and put into boiling water and boil the 10min enzyme that goes out; The tangerine peel that goes out behind the enzyme places the flowing water rinsing to colourless, uses kibbler to be crushed to the tangerine peel particle of particle diameter as 1-5mm then;
(2), acid hydrolysis
Get step (1) with the tangerine peel particle after pulverizing; By itself and the calculating of the mass ratio of water; Be the tangerine peel particle: water is that 1:20 mixes the back and uses concentration to regulate as the hydrochloric acid soln of 5mol/L that the pH value is 1.5, controlled temperature is 80 ℃ of extraction 75min after-filtration, and filtrating is carried out rotary evaporation in vacuo, obtain liquid concentrator after; The absolute ethyl alcohol that adds 3-5 times of volume again, suction filtration behind the deposition 1h;
(3), drying
The filter cake that obtains behind step (2) suction filtration is carried out drying respectively under 40 ℃ of the temperature, finally obtain the high ester pectin of 5.75g.
The yield of the high ester pectin of above-mentioned gained is 28.73%.This shows the tangerine peel particle: water is 1:20, and extracting temperature is 80 ℃, and extraction time is under the condition of 75min, can obtain maximum pectin yield.
Each item performance index of facing the high ester pectin of working method gained of the present invention are down verified
(1), the checking of gellifying property
Get the high ester pectin of the foregoing description 5 gained and each 0.5g of high ester pectin (commercially available homemade high ester pectin is available from Quzhou, Zhejiang pectin factory, and commercially available import high ester pectin is available from U.S. cpkelco company) of commercially available homemade and commercially available import, respectively with the dry mixing of 2.5g Icing Sugar; Behind the mixing; 80 ℃ the hot water that adds 49mL more respectively, treat that high ester pectin dissolves fully after, respectively add the Icing Sugar of 51.6g again; Process sugared concentration respectively and be 55% high ester pectin solution, be stirred to sugar and dissolve fully.The citric acid solution of preparation 0.5mol/L, the citric acid solution of measuring 1mL respectively form gel after 24h is placed in the back that stirs in each above-mentioned high ester pectin solution.Experiment adopts TA-XT plus matter structure appearance (available from Britain Stable Micro System company) to measure the performance of gel, and the result sees table 1.
The comparison of the gellifying property of the high ester pectin of table 1, commercially available homemade, commercially available import high ester pectin and embodiment 5 gained
| ? | Hardness/g | Viscosity/g.sec | Elasticity | Chewiness |
| Import | 13.796 | 0.000 | 0.857 | 2.269 |
| Homemade | 9.150 | 0.000 | 0.865 | 2.659 |
| Self-control | 12.258 | 0.554 | 0.783 | 4.353 |
Can find out by table 1; The chewability of the high ester pectin of embodiments of the invention 5 gained all is higher than commercially available import high ester pectin and commercially available homemade high ester pectin; It is thus clear that the high ester pectin chewiness of working method gained of the present invention is better; Can be used for soft sweets etc. has the making of the food of the strength of chewing, and secondly the hardness of the high ester pectin of working method gained of the present invention is higher than commercially available homemade high ester pectin, and a little less than commercially available import high ester pectin.
(2), the checking of rheological property
1., under concentration of the same race, the comparison of the rheological property of the high ester pectin of commercially available homemade, commercially available import high ester pectin (commercially available homemade high ester pectin is available from Quzhou, Zhejiang pectin factory, and commercially available import high ester pectin is available from U.S. cpkelco company) and embodiment 5 gained
Get each 0.5g of high ester pectin of commercially available homemade, commercially available import high ester pectin and embodiment 5 gained; Be dissolved in respectively in the hot water of 50mL, being mixed with concentration respectively is the high ester pectin solution of 1.00% commercially available homemade high ester pectin solution, commercially available import high ester pectin solution and embodiment 5 gained, after the dissolving fully; After treating 24h; Use the viscosity and the shear rate curve of each high ester pectin solution of AR-G2 type rheometer measurement, the result sees shown in Figure 1, and self-control HM pectin is the high ester pectin of embodiment 5 gained among Fig. 1; Homemade HM pectin is commercially available homemade high ester pectin, and import HM pectin is commercially available import high ester pectin.
Can find out under same concentrations, by Fig. 1 at 100-800s
-1In the range of shear rate, the viscosity of commercially available homemade high ester pectin is maximum, secondly is the high ester pectin of embodiments of the invention 5 gained, and what viscosity was minimum is commercially available import high ester pectin.
The high ester pectin of wherein commercially available homemade high ester pectin and embodiments of the invention 5 gained reduces along with shearing rate increases viscosity gradually, and the phenomenon of pseudoplastic fluid is apparent in view, and commercially available import high ester pectin has then presented the characteristic of Newtonian fuid.Can get thus, receive shear rate change minimum be commercially available import high ester pectin, secondly be the high ester pectin of embodiments of the invention 5 gained, receive the commercially available homemade high ester pectin that is that it has the greatest impact.
2., in the uniform temp variation range; The comparison of the rheological property of the high ester pectin of embodiments of the invention 5 gained, commercially available homemade high ester pectin and commercially available import high ester pectin (commercially available homemade high ester pectin is available from Quzhou, Zhejiang pectin factory, and commercially available import high ester pectin is available from U.S. cpkelco company)
The high ester pectin preparation high ester pectin concentration of getting the foregoing description 5 gained is 1.0% high ester pectin solution; After the dissolving fully; After treating 24h, with the viscosity of the high ester pectin solution of the AR-G2 type rheometer measurement embodiment of the invention 5 gained with receive the Influence of Temperature curve, its result sees shown in Figure 2.
The high ester pectin of working method gained as can be seen from Figure 2 of the present invention is along with the rising of temperature, viscosity degradation, but reduce under 25 ℃ the situation k value in the time of recovering with original 25 ℃ by 80 ℃.
Get commercially available homemade high ester pectin 0.5g; The preparation concentration of pectin is 1.0% pectin solution, after the dissolving fully, treat 24h after; With the viscosity of the formed commercially available homemade high ester pectin solution of AR-G2 type rheometer measurement with receive the Influence of Temperature curve, its result sees shown in Figure 3.
As can be seen from Figure 3 homemade high ester pectin can be along with the rising of temperature, differs greatly when viscosity degradation, but reduce under 25 ℃ the situation by 80 ℃, the k value of homemade high ester pectin and original 25 ℃.
Get commercially available import high ester pectin 0.5g; Preparation high ester pectin concentration is 1.0% commercially available import pectin solution, after the dissolving fully, treat 24h after; With the viscosity of the formed commercially available import high ester pectin solution of AR-G2 type rheometer measurement with receive the Influence of Temperature curve, its result sees shown in Figure 4.
As can be seen from Figure 4 commercially available import high ester pectin all can be along with the rising of temperature, and viscosity degradation is reduced under 25 ℃ the situation by 80 ℃, and is the most approaching when the k value of commercially available import high ester pectin can recover with original 25 ℃.
In sum; In identical range of temperature; The high ester pectin of working method gained of the present invention, commercially available homemade high ester pectin and commercially available import high ester pectin all can be along with the risings of temperature, viscosity degradation, but reduce under 25 ℃ the situation by 80 ℃; K value in the time of recovering with original 25 ℃ is immediate for the import high ester pectin, secondly is the high ester pectin of working method gained of the present invention.
In addition; The high ester pectin finished product each side gellifying property of working method gained of the present invention all is superior to the performance of commercially available homemade pectin; When the high ester pectin strength of solution that forms is higher, show as pseudoplastic fluid, and along with the rising of temperature; Its viscosity reduces gradually, more approaches the high ester pectin of commercially available import.
The above content is merely the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (5)
1. the working method of the high ester pectin of an intermittent type acid extraction ethanol sedimentation is characterized in that comprising the following steps:
(1), the pre-treatment of tangerine peel
Take by weighing dried tangerine peel 20g, be soaked in 30min in 45 ℃ of warm water, it is softening that it is fully absorbed water; Remove soluble impurity; Drain tangerine peel and put into boiling water and boil the 10min enzyme that goes out, the tangerine peel behind the enzyme that goes out places the flowing water rinsing to colourless, uses kibbler to be crushed to the tangerine peel particle of particle diameter as 1-5mm then;
(2), acid hydrolysis
Get step (1) with the tangerine peel particle after pulverizing; By itself and the calculating of the mass ratio of water; Be the tangerine peel particle: water be 1:5-20 mix the back uses concentration as the hydrochloric acid soln of 5mol/L regulate the pH value as 1.0-3.0, controlled temperature as 50-90 ℃ of extraction 30-90min after-filtration, filtrating is carried out rotary evaporation in vacuo, obtain liquid concentrator after; The absolute ethyl alcohol that adds 3-5 times of volume again, suction filtration behind the deposition 1h;
(3), drying
The filter cake that obtains behind step (2) suction filtration is carried out drying under 40 ℃ of temperature, finally obtain high ester pectin.
2. the working method of the high ester pectin of a kind of intermittent type acid extraction ethanol sedimentation as claimed in claim 1 is characterized in that step (1) described extraction time is 75min.
3. the working method of the high ester pectin of a kind of intermittent type acid extraction ethanol sedimentation as claimed in claim 2 is characterized in that the described extraction temperature of step (2) is 80 ℃.
4. the working method of the high ester pectin of a kind of intermittent type acid extraction ethanol sedimentation as claimed in claim 3 is characterized in that the described pH value of step (2) is 1.5.
5. the working method of the high ester pectin of a kind of intermittent type acid extraction ethanol sedimentation as claimed in claim 4 is characterized in that the described tangerine peel particle of step (2), and by itself and the calculating of the mass ratio of water, i.e. tangerine peel particle: water is 1:20.
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| CN104974274A (en) * | 2015-07-01 | 2015-10-14 | 安徽亿源生物工程有限公司 | Preparation method of high esterification degree super slow set pectin |
| CN105061634A (en) * | 2015-07-01 | 2015-11-18 | 安徽亿源生物工程有限公司 | Method for preparing pectin through double-effect combined extraction technology |
| CN105242019A (en) * | 2015-09-24 | 2016-01-13 | 苏州泽达兴邦医药科技有限公司 | Traditional Chinese medicine alcohol precipitation technological process pH on-line detection method |
| CN107629144A (en) * | 2017-11-13 | 2018-01-26 | 何会平 | The method that sugar orange cull fruit extracts pectin |
| CN110396141A (en) * | 2019-08-19 | 2019-11-01 | 华南理工大学 | A method of preparing the high-ester pectin of purpose esterification degree |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104974274A (en) * | 2015-07-01 | 2015-10-14 | 安徽亿源生物工程有限公司 | Preparation method of high esterification degree super slow set pectin |
| CN105061634A (en) * | 2015-07-01 | 2015-11-18 | 安徽亿源生物工程有限公司 | Method for preparing pectin through double-effect combined extraction technology |
| CN105242019A (en) * | 2015-09-24 | 2016-01-13 | 苏州泽达兴邦医药科技有限公司 | Traditional Chinese medicine alcohol precipitation technological process pH on-line detection method |
| CN107629144A (en) * | 2017-11-13 | 2018-01-26 | 何会平 | The method that sugar orange cull fruit extracts pectin |
| CN110396141A (en) * | 2019-08-19 | 2019-11-01 | 华南理工大学 | A method of preparing the high-ester pectin of purpose esterification degree |
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