CN103923225A - Method for preparing citrus pectin - Google Patents
Method for preparing citrus pectin Download PDFInfo
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- CN103923225A CN103923225A CN201410168320.8A CN201410168320A CN103923225A CN 103923225 A CN103923225 A CN 103923225A CN 201410168320 A CN201410168320 A CN 201410168320A CN 103923225 A CN103923225 A CN 103923225A
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Abstract
The invention relates to a method for preparing citrus pectin. The method comprises the following steps: (1) weighing citrus raw materials, cleaning, rubbing and drying; (2) crushing, screening, and adding 5-15 times by volume of alcohol solution for extraction; (3) squeezing and filtering, adding 5-15 times by volume of water in the filter residues to regulate the pH to 2-4; (4) carrying out a high voltage pulsed electric field treatment, intermittent heating extraction, centrifuging, repeatedly carrying out the treatment for multiple times, mixing the filtrate, concentrating, adding an acidic alcohol solution, standing and suction filtrating; (5) adding 95% ethanol in the precipitate, suction filtrating, drying, crushing, and sieving through a sieve of 60 meshes to obtain a finished product of citrus pectin. The method can be used for not only greatly improving the yield and quality of the citrus pectin and shortening the production cycle, but also reducing the energy consumption and the environmental pollution.
Description
Technical field
The present invention relates to the preparation of a kind of pectin in natural product manufacture field, be specifically related to a kind of preparation method of citrus pectin.
Background technology
Pectin is a kind of colloidality polysaccharide compound, and its basic structure is that main chain connects with Isosorbide-5-Nitrae-glycosidic link with β-D-pyrans aldehydic acid, and side chain is the O at L-rhamnosyl residue
4upper with α-1,2-glycosidic link connects β-1, the semi-lactosi of 2-glycosidic link, and its molecular formula is (C
6h
10o
7)
n.Conventionally exist with part esterification state, molecular weight is 10000～400000, and the corresponding polymerization degree exceedes 1,000 unit.Pectin is present in the cell walls of leaf, root, stem, fruit of higher plant, sticks together each other with vegetable cell, and especially the massfraction in fruit and leaf is more, and pectin is the main component that middle lamella is adhered cell.
Pectin is widely used in foodstuffs industry, can be used as jelling agent, in the making of jelly, jam, soft sweets etc. in yoghurt product, pectin can improve its local flavor, also can play stable and freshening effect, prevent the floating and coagulation of casein of pulp in yogurt, extend yoghurt product open date.Pectin, as foodstuff additive, by the evaluation of FAO/WHO foodstuff additive joint committee, announce that it is nontoxic, and addition is unrestricted.
Pectin is also a lot of in medicine, filed of daily-use chemical industry application, as it has good curative effect to hypertension, intestinal cancer, obesity, can suppress Human colon cancer and leukemia cell's hyperplasia.Pectin can also reduce serum cholesterol, blood-sugar content, and preventing cancer occurs and shifts, and prevents that heavy metal ion is poisoning, especially lead poisoning.In addition, pectin can not only reduce cholesterol, also has anti-oxidant activity, and pectin after hydroximic acid modification, and the natural pectin of Green Tea Extract specific activity is stronger.
The preparation method of pectin has much at present, industrial production pectin is modal is classical acid formulation, utilizes dilute acid soln that non-water-soluble protopectin-is changed into water soluble pectin, then adds alcohol or polyvalent metal salt, separate out pectin precipitation, make pectin finished product through washing, be dried, pulverizing.Classical acid formulation technique is simple, with low cost, but owing to being subject to the impact of extraction conditions larger, efficiency is lower, and the production cycle is also longer.
Summary of the invention
The object of this invention is to provide a kind of preparation method of citrus pectin, adopt the method can not only significantly improve pectin yield and quality, shorten the production cycle, can also reduce energy consumption and environmental pollution.
The object of the invention is to be achieved through the following technical solutions:
A preparation method for citrus pectin, described preparation method comprises the following steps:
1. take oranges and tangerines as raw material, clean up rear rubbing, dry;
2. the raw material after step being dried in is 1. pulverized, and crosses 40-80 mesh sieve, and adds raw material volume 5-15 alcoholic solution doubly, 60-80 DEG C of lixiviate 1-4h;
8. by step 2. in the raw material of lixiviate carry out squeeze and filter, filter residue adds the water of 5-15 times of volume, and is adjusted to PH2-4 with hydrochloric acid;
4. adopt pulsed electric field processing, intermittent type heating is extracted, centrifugal, is so cycled to repeat 2～4 times, preferably repeats 3 times, and merging filtrate, and filtrate is concentrated, to the acidity alcohol solution that adds 1-5 times of volume in concentrated solution, leaves standstill 2-6h, suction filtration;
5. add 95% ethanol in precipitation after suction filtration in step in 4. and stir 10min, suction filtration, carries out vacuum-drying by being deposited at 45 DEG C of obtaining, pulverizes, and crosses 60 mesh sieves, obtains citrus pectin finished product.
Further, step 1. described oranges and tangerines be oranges and tangerines cull fruit or orange food processing waste material.
Further, step 1. described dry temperature be 60-80 DEG C.
Further, the alcoholic solution of step described in is 2. 40%-100% alcoholic solution.
Further, described alcoholic solution is 60%-75% ethanolic soln
Further, the strength of electric field of the pulsed electric field of step described in is 4. 10 to 24kV/cm, and umber of pulse is 5～12, and temperature is 40-80 DEG C.
Further, the intermittent type heating of step described in 4. extracted detailed process and is: the processing of advanced horizontal high voltage pulsed electrical field, and then carry out insulated and stirred extraction, and the temperature that described insulated and stirred is extracted is 40-80 DEG C, the time that insulated and stirred is extracted is 10-60min.
Further, step 4. in to the acidity alcohol solution that adds while stirring 2-4 times of volume in concentrated solution.
Further, the described acidity alcohol solution of step described in is 4. the alcoholic solution containing 0.5mol/L HC1.
Further, described alcoholic solution is 95% ethanolic soln.
The invention provides a kind of preparation method of citrus pectin, its beneficial effect mainly having is.
1. the present invention is applied to pulsed electric field treatment technology in the leaching process of pectin, adopt intermittent high-pressure pulsed electrical field auxiliary acid formulation, in definite strength of electric field, umber of pulse and temperature range, can extract fast and effectively pectin, pectin yield and stay in grade.
2. in addition, the inventive method is carried out alcohol processing and can effectively be removed the impurity such as pigment and lipid composition by extracting front raw material, is conducive to the carrying out of subsequent handling, is conducive to improve the quality of pectin product.
3. the inventive method is simple to operation, and extraction efficiency is high, is applicable to suitability for industrialized production, the extraction time that has solved traditional pectin extraction method existence is long, and production efficiency is low, and pectin yield is low, pectin poor quality, the problem such as unstable, is conducive to improve the competitive power of pectin product on market.
4. method of the present invention has important industrial market using value, and this pectin product can be widely used in food, healthcare products, makeup, medicine and other fields.
Embodiment
The preparation method of a kind of citrus pectin described in the embodiment of the present invention, described preparation method comprises the following steps: 1. take oranges and tangerines as raw material, clean up rear rubbing, dry; 2. the raw material after step being dried in is 1. pulverized, and crosses 40-80 mesh sieve, and adds the alcoholic solution of 5-15 times of volume, 60-80 DEG C of lixiviate 1-4h; 3. by step 2. in the raw material of lixiviate carry out squeeze and filter, filter residue adds the water of 5-15 times of volume, and is adjusted to PH2-4 with hydrochloric acid; 4. adopt pulsed electric field processing, intermittent type heating is extracted, centrifugal, is so cycled to repeat 2～4 times, and merging filtrate, and filtrate is concentrated, to the acidity alcohol solution that adds 1-5 times of volume in concentrated solution, leaves standstill 2-6h, suction filtration; 5. add 95% ethanol in precipitation after suction filtration in step in 4. and stir 10min, suction filtration, carries out vacuum-drying by being deposited at 45 DEG C of obtaining, pulverizes, and crosses 60 mesh sieves, obtains citrus pectin finished product.
As further preferably, step 1. described oranges and tangerines is oranges and tangerines cull fruit or orange food processing waste material.
As further preferably, step 1. described dry temperature is 60-80 DEG C.
As further preferably, the alcoholic solution of step described in is 2. 40%-100% alcoholic solution.
As further preferably, described alcoholic solution is 60%-75% ethanolic soln
As further preferably, the strength of electric field of the pulsed electric field of step described in is 4. 10 to 24kV/cm, and umber of pulse is 5～12, and temperature is 40-80 DEG C.
As further preferably, the intermittent type heating of step described in 4. extracted detailed process and is: the processing of advanced horizontal high voltage pulsed electrical field, and then carry out insulated and stirred extraction, and the temperature that described insulated and stirred is extracted is 40-80 DEG C, the time that insulated and stirred is extracted is 10-60min.
As further preferably, step 4. in to the acidity alcohol solution that adds while stirring 2-4 times of volume in concentrated solution.
As further preferably, the described acidity alcohol solution of step described in is 4. the alcoholic solution containing 0.5mol/L HC1.
As further preferably, described alcoholic solution is 95% ethanolic soln.
When concrete enforcement, pulsed electric field is a kind of non-heat treatment technics, aspect processing heat-sensitive substance, has huge advantage.Pulsed electric field can utilize high potential gradient to destroy plant cell membrane, can not only make the inactivations such as desmo enzyme class material, can also significantly increase intracellular matter stripping.
As an example of specific experiment case example, embodiment is described below, should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Embodiment 1
Get oranges and tangerines raw material, clean up rear rubbing, 65-75 DEG C of oven dry, pulverizes, and crosses 40-80 mesh sieve, adds 70% ethanolic soln of 15 times of volumes, 75-80 DEG C of lixiviate 1h, and squeeze and filter, filter residue adds the water of 12 times of volumes, with hydrochloric acid tune PH to 2, use again pulsed electric field processing, the strength of electric field of this pulsed electric field processing is 10kV/cm, umber of pulse is 10, temperature is 60 DEG C, after pulsed electric field is processed, keep temperature 60 C stirring heating to extract 30min, centrifugal, so be cycled to repeat 3 times, merging filtrate, filtrate is concentrated, to 95% ethanolic soln containing 0.5mol/L HC1 that adds while stirring equal volume amounts in concentrated solution, leave standstill 2h, suction filtration, gained precipitation adds 95% ethanol and stirs 10min, suction filtration, being deposited in of obtaining carried out to vacuum-drying at 45 DEG C, pulverize and cross 60 mesh sieves, obtain citrus pectin finished product.
Embodiment 2
Get oranges and tangerines raw material, clean up rear rubbing, 60-70 DEG C of oven dry, pulverizes, and crosses 40-80 mesh sieve, adds 80% ethanolic soln of 10 times of volumes, 60-70 DEG C of lixiviate 3h, and squeeze and filter, filter residue adds the water of 10 times of volumes, with hydrochloric acid tune PH to 3, use again pulsed electric field processing, the strength of electric field of this pulsed electric field processing is 15kV/cm, umber of pulse is 12, temperature is 80 DEG C, after pulsed electric field is processed, keep 80 DEG C of stirring heating of temperature to extract 40min, centrifugal, so be cycled to repeat 3 times, merging filtrate, filtrate is concentrated, to 95% ethanolic soln containing 0.5mol/L HC1 that adds while stirring 2 times of volumes in concentrated solution, leave standstill 3～5h, suction filtration, gained precipitation adds 95% ethanol and stirs 10min, suction filtration, being deposited in of obtaining carried out to vacuum-drying at 45 DEG C, pulverize and cross 60 mesh sieves, obtain citrus pectin finished product.
Embodiment 3
Get oranges and tangerines raw material, clean up rear rubbing, 70-80 DEG C of oven dry, pulverizes, and crosses 40-80 mesh sieve, adds 60% ethanolic soln of 6 times of volumes, 75-80 DEG C of lixiviate 1.5h, and squeeze and filter, filter residue adds the water of 15 times of volumes, with hydrochloric acid tune PH to 4, use again pulsed electric field processing, the strength of electric field of this pulsed electric field processing is 20kV/cm, umber of pulse is 8, temperature is 40 DEG C, after pulsed electric field is processed, keep 40 DEG C of stirring heating of temperature to extract 45min, centrifugal, so be cycled to repeat 3 times, merging filtrate, filtrate is concentrated, to 95% ethanolic soln containing 0.5mol/L HC1 that adds while stirring 3 times of volumes in concentrated solution, leave standstill 4.5h, suction filtration, gained precipitation adds 95% ethanol and stirs 10min, suction filtration, being deposited in of obtaining carried out to vacuum-drying at 45 DEG C, pulverize and cross 60 mesh sieves, obtain citrus pectin finished product.
The present invention is not limited to above-mentioned preferred forms, any modification relevant of the present invention or change that anyone does under enlightenment of the present invention, and every have identical with a application or akin technical scheme, within all dropping on protection scope of the present invention.
Claims (10)
1. a preparation method for citrus pectin, is characterized in that: described preparation method comprises the following steps:
1. take oranges and tangerines as raw material, clean up rear rubbing, dry;
2. the raw material after step being dried in is 1. pulverized, and crosses 40-80 mesh sieve, and adds the alcoholic solution of 5-15 times of volume, 60-80 DEG C of lixiviate 1-4h;
3. by step 2. in the raw material of lixiviate carry out squeeze and filter, filter residue adds the water of 5-15 times of volume, and is adjusted to PH2-4 with hydrochloric acid;
4. adopt pulsed electric field processing, intermittent type heating is extracted, centrifugal, is so cycled to repeat 2～4 times, and merging filtrate, and filtrate is concentrated, to the acidity alcohol solution that adds 1-5 times of volume in concentrated solution, leaves standstill 2-6h, suction filtration;
5. add 95% ethanol in precipitation after suction filtration in step in 4. and stir 10min, suction filtration, carries out vacuum-drying by being deposited at 45 DEG C of obtaining, pulverizes, and crosses 60 mesh sieves, obtains citrus pectin finished product.
2. the preparation method of citrus pectin according to claim 1, is characterized in that: step 1. described oranges and tangerines is oranges and tangerines cull fruit or orange food processing waste material.
3. the preparation method of citrus pectin according to claim 1, is characterized in that: step 1. described dry temperature is 60-80 DEG C.
4. the preparation method of citrus pectin according to claim 1, is characterized in that: the alcoholic solution of step described in is 2. 40%-100% alcoholic solution.
5. the preparation method of citrus pectin according to claim 4, is characterized in that: described alcoholic solution is 60%-75% ethanolic soln.
6. the preparation method of citrus pectin according to claim 1, is characterized in that: the strength of electric field of the pulsed electric field of step described in is 4. 10 to 24kV/cm, and umber of pulse is 5～12, and temperature is 40-80 DEG C.
7. the preparation method of citrus pectin according to claim 1, it is characterized in that: the intermittent type heating of step described in 4. extracted detailed process and be: the processing of advanced horizontal high voltage pulsed electrical field, and then carry out insulated and stirred extraction, the temperature that described insulated and stirred is extracted is 40-80 DEG C, and the time that insulated and stirred is extracted is 10-60min.
8. the preparation method of citrus pectin according to claim 1, is characterized in that: step 4. in to the acidity alcohol solution that adds while stirring 2-4 times of volume in concentrated solution.
9. the preparation method of citrus pectin according to claim 8, is characterized in that: the described acidity alcohol solution of step described in is 4. the alcoholic solution containing 0.5mol/L HC1.
10. the preparation method of citrus pectin according to claim 9, is characterized in that: described alcoholic solution is 95% ethanolic soln.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108285499A (en) * | 2017-12-03 | 2018-07-17 | 新疆阜丰生物科技有限公司 | A kind of energy-efficient technique for preparing pectin |
| CN108424940A (en) * | 2018-04-13 | 2018-08-21 | 安徽宇宁果胶股份有限公司 | A kind of production method of the medicinal pectin of targeted therapy |
| WO2019061018A1 (en) * | 2017-09-26 | 2019-04-04 | 浙江大学 | Method for extracting pectin rich in rg-i |
| CN114685690A (en) * | 2022-04-08 | 2022-07-01 | 江南大学 | Method for extracting edible fungus polysaccharide by using intermittent induction thermal reactor |
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| JP2010116524A (en) * | 2008-11-14 | 2010-05-27 | Asukii:Kk | Extraction method for polysaccharide |
| CN102702379A (en) * | 2012-04-26 | 2012-10-03 | 赛珂睿德生物医药科技(上海)有限公司 | Extraction and preparation process of citrus pectin |
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| JP2010116524A (en) * | 2008-11-14 | 2010-05-27 | Asukii:Kk | Extraction method for polysaccharide |
| CN102702379A (en) * | 2012-04-26 | 2012-10-03 | 赛珂睿德生物医药科技(上海)有限公司 | Extraction and preparation process of citrus pectin |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019061018A1 (en) * | 2017-09-26 | 2019-04-04 | 浙江大学 | Method for extracting pectin rich in rg-i |
| US11292852B2 (en) | 2017-09-26 | 2022-04-05 | Zhejiang University | Method for extracting RG-I-rich pectin |
| CN108285499A (en) * | 2017-12-03 | 2018-07-17 | 新疆阜丰生物科技有限公司 | A kind of energy-efficient technique for preparing pectin |
| CN108424940A (en) * | 2018-04-13 | 2018-08-21 | 安徽宇宁果胶股份有限公司 | A kind of production method of the medicinal pectin of targeted therapy |
| CN114685690A (en) * | 2022-04-08 | 2022-07-01 | 江南大学 | Method for extracting edible fungus polysaccharide by using intermittent induction thermal reactor |
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Effective date of registration: 20170119 Address after: 215123 Jiangsu Province Industrial Park of Suzhou Dushu Lake higher education if the waterway No. 398 Patentee after: Love Kang biological medicine (Suzhou) Co., Ltd. Patentee after: Saccharidia Bio-Pharmaceutical Technology (Shanghai) Co., Ltd. Address before: 201203 Shanghai city Pudong New Area Cailun Road No. 781 room 1204 Patentee before: Saccharidia Bio-Pharmaceutical Technology (Shanghai) Co., Ltd. |