CN112457431A - Production method of dry and wet raw material blended pectin - Google Patents
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- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
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Abstract
The invention relates to a method for producing pectin by blending dry and wet raw materials, which is simple and effective, can be used for co-production with a juice squeezing or essential oil production line, can utilize the same production line, is not limited by the raw material quantity, and can stably produce pectin. Fully utilizes other production lines for producing the fresh fruit peel and peel residues to solve the problems that the amount of the fresh fruit peel and peel residues is not enough and the fresh fruit peel and peel residues can not be preserved. By combining the proportion of different ingredients and the treatment method, the yield of the pectin produced by the dry and wet materials is improved, the extracting solution is fully utilized, and the discharge of the extracted waste water is reduced.
Description
Technical Field
The invention belongs to the technical field of agricultural byproduct reprocessing, and relates to a method for producing pectin by blending dry and wet raw materials.
Background
Pectin is a type of heteropolysaccharide widely present in the primary wall and the middle layer of plant cell wall and composed of D-Galacturonic acid (D-Galactonic Acids, D-Gal-A) connected by alpha-1, 4-glycosidic bonds. Pectin has good gelling and emulsifying stabilizing effects, and can be widely used in food, medicine and cosmetic industries.
The pectin material is obtained from a wide variety of sources, and can be extracted from apple, citrus and orange peel residues, beet residue, sunflower tray and stem, papaya, watermelon peel, sea buckthorn and pumpkin. At present, commercial pectin is produced by using apple peel residue, citrus, lemon or orange peel residue as a main raw material, and pectin is extracted from byproducts such as banana peel, sunflower, sweet potato, premna microphylla leaf and the like, but the research on the raw materials is still basically in basic research in a laboratory at present. The pectin content and monosaccharide composition in different raw materials differ greatly, so the preparation processes using different raw materials are also different. In general industrial production lines, single substances are used as raw materials. The production line is single, is greatly influenced by the source of raw materials, particularly is a production line which is co-produced with production lines of fruit juice, essential oil and the like and takes the fresh fruit peel and peel residues as the raw materials, is sometimes influenced by the yield of the fresh fruit peel and peel residues, and cannot be used for the production line of primary quantitative equipment. The fresh fruit peel residue has short fresh-keeping time, is more prone to decay and deteriorate than fresh fruits, and wastes time and labor when being prepared into dry peel.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for producing pectin by blending dry and wet raw materials, which effectively and fully utilizes the reprocessing production line of oranges, lemons or oranges.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a method for producing pectin by blending dry and wet raw materials comprises the following steps:
1) adding water into dried lemon peel, performing ultrasonic cleaning at a material-liquid ratio of 1:10-20(W/W), performing solid-liquid separation, and extracting with nitric acid water at pH of 1.0-2.8 at an extraction material-liquid ratio of 1:20-40 for 1-1.5 hr;
2) the method comprises the following steps of crushing wet lemon peels, adding water for ultrasonic cleaning, wherein the material-liquid ratio by mass in cleaning is 1:3-8 (W/W), performing solid-liquid separation, squeezing until the water content is less than 75%, and repeating the cleaning once;
3) after the extraction reaction of the dried lemon peel is carried out for 1 to 1.5 hours, adding the prepared wet raw material in the step 2) until the material-liquid ratio is 1:3-8, adding nitric acid to adjust the pH value to be 1.0 to 2.8, and continuing the extraction reaction for 2 to 4 hours; then adding ammonia water to adjust the pH value to 2.8-3.2 to terminate the reaction; performing solid-liquid separation to obtain primary extract;
4) performing ion exchange on the primary extract with cation exchange resin at pH2.8-3.2 and pH 60-75% in an amount of 10-30% for 100-120 min.
Preferably, the ultrasonic water cleaning feed-liquid ratio in the step 1) is 1:10-12 (W/W).
Preferably, the extracting solution in the step 1) is nitric acid water with the pH value of 1.1-2.4, and the material-liquid ratio is 1: 20-30.
Preferably, the ratio of the cleaning materials to the cleaning liquid in the step 2) is 1: 3-4(W/W), adding nitric acid to adjust the pH value to 1.1-2.4.
Preferably, in the step 3), the solid-liquid separation is performed by coarse filtration by a plate-and-frame filter press and fine filtration by a leaf filter.
Preferably, the dosage of the cation exchange resin in the step 4) is 15-25%.
Preferably, the pectin production process further comprises the step 5) of precipitating: concentrating the liquid subjected to ion exchange in the step 4) by 3.8-4.5 times by using an evaporator to obtain concentrated solution, wherein the evaporation temperature is 70-88 ℃; precipitating with 70-80% ethanol at a volume ratio of concentrated solution to ethanol of 1:2-1:2.6 (V/V).
Preferably, the pectin production process further comprises step 6): performing solid-liquid separation on the precipitate obtained in the step 5), adding 75-80% ethanol into the separated solid matter, and cleaning for the first time, wherein the content of the suspended solid matter is 0.7-2.5% (V/V); solid-liquid separation, adding 80-88% ethanol into the separated solid matter for secondary cleaning, wherein the content of the suspended solid matter is 0.5-2.2% (V/V); and (4) performing solid-liquid separation and drying.
Preferably, the solid-liquid separation drying is washing and pressure filtering to obtain pectin solid with dry matter content higher than 45%, spraying 5% sodium carbonate water solution to adjust pH to be higher than 3.0, drying until water content is lower than 10%, and drying with boiling dryer at 85-95 deg.C for 1.5-2.5 hr; pulverizing to 60-80 mesh.
The invention has the beneficial effects that: the pectin production method by blending dry and wet raw materials can ensure the co-production with lemon juice, essential oil and other production lines, and fully utilizes other production lines for producing fresh peel and peel residues, so as to solve the problems of insufficient fresh peel and peel residues and incapability of storing the fresh peel and peel residues. By combining the proportion of different ingredients and the treatment method, the yield of the pectin produced by the dry and wet materials is improved, the extracting solution is fully utilized, and the discharge of the extracted waste water is reduced.
Detailed Description
The preferred embodiments of the present invention will be described in detail below. The experimental procedures, in which specific conditions are not specified in the examples, are generally carried out under conventional conditions or under conditions recommended by the manufacturers.
A method for producing pectin by blending dry and wet raw materials comprises the following steps:
1) weighing dried raw materials (dried lemon peels), adding water, performing ultrasonic cleaning for 15-30min, wherein the material-liquid ratio is 1:10-20(W/W) by mass, performing solid-liquid separation, and then putting into an extraction tank for extraction, wherein the extract is nitric acid water (the pH value is adjusted to 1.0-2.8 by 65-68% nitric acid), the material-liquid ratio is 1:20-40, and the extraction is performed for 1-1.5 hours; preferably, the ultrasonic water cleaning feed-liquid ratio is 1:10-12 (W/W); preferably, the extracting solution is nitric acid water with the pH value of 1.1-2.4, and the material-liquid ratio is 1: 20-30.
2) Simultaneously preparing wet raw materials (wet lemon peels after juicing or essential oil extraction), firstly crushing to 1-3mm, weighing, adding water, and carrying out ultrasonic cleaning for 15-30min, wherein the material-liquid ratio by mass in cleaning is 1:3-8 (W/W), performing solid-liquid separation, squeezing to water content of less than 75%, and repeating the washing once. Preferably, the ratio of cleaning materials to liquid is 1: 3-4 (W/W). The method comprises the steps of respectively treating the dry raw materials and the wet raw materials according to component differences, screening a large number of suitable proportions, reducing the use and discharge of nitric acid in an extracting solution, improving the efficiency of subsequent treatment and improving the extraction rate of pectin.
3) After the dry raw materials are subjected to extraction reaction for 1-1.5 hours, adding the wet raw materials prepared in the step 2) until the material-liquid ratio is 1:3-8, adding 65-68% nitric acid to adjust the pH value to be 1.0-2.8, and continuously performing extraction reaction for 2-4 hours; adding 22-25% ammonia water to adjust pH to 2.8-3.2 to terminate the reaction; separating solid and liquid to obtain primary extract, performing coarse filtration with plate and frame filter press, and fine filtration with leaf filter; preferably, nitric acid is added to adjust the pH to 1.1-2.4.
4) Performing ion exchange on the primary extracting solution by using 711 cation exchange resin, wherein the dosage of the cation exchange resin is 10-30 percent, namely the weight is the percentage of the total mass of the dry raw material and the wet raw material, and the weight is the same as the weight of the dry raw material and the wet raw material; pH2.8-3.2, temperature 60-75 deg.C, and time 100-120 min; the preferred amount of cation exchange resin is 15% to 25%.
5) And (3) precipitation: concentrating the liquid subjected to ion exchange in the step 4) by 3.8-4.5 times by using an evaporator to obtain concentrated solution, wherein the evaporation temperature is 70-88 ℃; precipitating with 70-80% ethanol at a volume ratio of concentrated solution to ethanol of 1:2-1:2.6 (V/V);
6) solid-liquid separation is carried out on the precipitate obtained in the step 5), the separated solid is added with 75-80% ethanol for the first time, and the content of the suspended solid is 0.7-2.5% (V/V); solid-liquid separation, adding 80-88% ethanol into the separated solid matter for secondary cleaning, wherein the content of the suspended solid matter is 0.5-2.2% (V/V); water-soluble impurities are removed by two times of cleaning, and the water content in pectin can be further reduced when the alcohol concentration is increased by the second cleaning.
7) Cleaning, press filtering to obtain pectin solid with dry matter content greater than 45%, spraying 5% sodium carbonate aqueous solution to adjust pectin pH to more than 3.0, drying until water content is less than 10%, and drying at 85-95 deg.C for 1.5-2.5 hr with boiling drier; pulverizing to 60-80 mesh.
Example 1
1) Weighing dry raw materials (dried lemon peels), adding water, performing ultrasonic cleaning for 15-30min, wherein the material-liquid ratio by mass is 1:12(W/W), performing solid-liquid separation, and then putting into an extraction tank for extraction, wherein an extracting solution is nitric acid water with the pH value of 1.9 (adjusted to the pH value of 1.9 by using 65-68% nitric acid), and the material-liquid ratio is 1:20, extracting for 1.5 hours;
2) simultaneously, preparing wet raw materials (wet lemon peels after juicing), crushing to 1-3mm, weighing, adding water, and performing ultrasonic cleaning for 15-30min, wherein the material-liquid ratio by mass in cleaning is 1: 4(W/W), performing solid-liquid separation and squeezing until the water content is less than 75%, and repeating the washing once;
3) after the dry raw materials are extracted and reacted for 1.5 hours, adding the wet raw materials prepared in the step 2) until the material-liquid ratio is 1:4, adding 65-68% nitric acid to adjust the pH value to 1.9, and continuing the extraction and reaction for 4 hours; adding 22-25% ammonia water to adjust pH to 2.8-3.2 to terminate the reaction; separating solid and liquid to obtain primary extract, performing coarse filtration with plate and frame filter press, and fine filtration with leaf filter;
4) performing ion exchange on the primary extracting solution by using 711 cation exchange resin, wherein the dosage of the cation exchange resin is 15 percent, namely the weight is the percentage of the total mass of the dry raw material and the wet raw material, and the weight is the same as the percentage; pH2.8-3.2, temperature 60-75 deg.C, and time 100 min;
5) and (3) precipitation: concentrating the liquid subjected to ion exchange in the step 4) by 4 times by using an evaporator to obtain a concentrated solution, wherein the evaporation temperature is 70-88 ℃; precipitating with 70-80% ethanol at a volume ratio of the concentrated solution to ethanol of 1:2.6 (V/V);
6) solid-liquid separation is carried out on the precipitate obtained in the step 5), the separated solid is added with 75-80% ethanol for the first time, and the content of the suspended solid is 2% (V/V); solid-liquid separation, adding 80-88% ethanol into the separated solid matter for secondary cleaning, and the content of the suspended solid matter is 2% (V/V);
7) cleaning, press filtering to obtain pectin solid with dry matter content greater than 45%, spraying 5% sodium carbonate aqueous solution to adjust pectin pH to more than 3.0, drying until water content is less than 10%, and drying at 85-95 deg.C for 1.5-2.5 hr with boiling drier; pulverizing to 60-80 mesh.
Example 2
1) Weighing dry raw materials (dried lemon peels), adding water, performing ultrasonic cleaning for 15-30min, wherein the material-liquid ratio by mass is 1:10(W/W), performing solid-liquid separation, and then putting into an extraction tank for extraction, wherein the extracting solution is nitric acid water with the pH value of 1.5 (adjusted to the pH value of 1.5 by using 65-68% nitric acid), the material-liquid ratio is 1:20, and extracting for 1 hour;
2) simultaneously, preparing wet raw materials (wet lemon peels after juicing), crushing to 1-3mm, weighing, adding water, and performing ultrasonic cleaning for 15-30min, wherein the material-liquid ratio by mass in cleaning is 1: 3(W/W), performing solid-liquid separation, squeezing until the water content is less than 75%, and repeating the washing once;
3) after the dry raw materials are extracted and reacted for 1 hour, adding the wet raw materials prepared in the step 2) until the material-liquid ratio is 1: 5, adding 65-68% nitric acid to adjust the pH value to 1.5, and continuing the extraction reaction for 2 hours; adding 22-25% ammonia water to adjust pH to 2.8-3.2 to terminate the reaction; separating solid and liquid to obtain primary extract, performing coarse filtration with plate and frame filter press, and fine filtration with leaf filter;
4) performing ion exchange on the primary extract by using 711 cation exchange resin, wherein the using amount of the cation exchange resin is 15%; pH2.8-3.2, temperature 60-75 deg.C, and time 100 min;
5) and (3) precipitation: concentrating the liquid subjected to ion exchange in the step 4) by 3.8-4.5 times by using an evaporator to obtain concentrated solution, wherein the evaporation temperature is 70-88 ℃; adding 70-80% ethanol for precipitation, wherein the volume ratio of the concentrated solution to the ethanol is 1:2 (V/V);
6) solid-liquid separation is carried out on the precipitate obtained in the step 5), the separated solid is added with 75-80% ethanol for the first time, and the content of the suspended solid is 1% (V/V); solid-liquid separation, adding 80-88% ethanol into the separated solid matter for secondary cleaning, and keeping the content of the suspended solid matter at 1% (V/V);
7) cleaning, press filtering to obtain pectin solid with dry matter content greater than 45%, spraying 5% sodium carbonate aqueous solution to adjust pectin pH to more than 3.0, drying until water content is less than 10%, and drying at 85-95 deg.C for 1.5-2.5 hr with boiling drier; pulverizing to 60-80 mesh.
Example 3
1) Weighing dried raw materials (dried lemon peels), adding water, performing ultrasonic cleaning for 15-30min, wherein the material-liquid ratio is 1:12(W/W) by mass, performing solid-liquid separation, and then putting into an extraction tank for extraction, wherein an extracting solution is nitric acid water with the pH value of 2.1 (adjusted to the pH value of 2.1 by using 65-68% nitric acid), the material-liquid ratio is 1:20-40, and the extraction is performed for 1-1.5 hours;
2) simultaneously, preparing wet raw materials (wet lemon peels after juicing), crushing to 1-3mm, weighing, adding water, and performing ultrasonic cleaning for 15-30min, wherein the material-liquid ratio by mass in cleaning is 1: 4(W/W), performing solid-liquid separation and squeezing until the water content is less than 75%, and repeating the washing once;
3) after the dry raw materials are extracted and reacted for 1-1.5 hours, adding the wet raw materials prepared in the step 2) until the material-liquid ratio is 1:3, adding 65-68% nitric acid to adjust the pH value to 2.1, and continuing the extraction reaction for 2-4 hours; adding 22-25% ammonia water to adjust pH to 2.8-3.2 to terminate the reaction; separating solid and liquid to obtain primary extract, performing coarse filtration with plate and frame filter press, and fine filtration with leaf filter;
4) performing ion exchange on the primary extract by using 711 cation exchange resin, wherein the using amount of the cation exchange resin is 20%; pH2.8-3.2, temperature 60-75 deg.C, and time 100-120 min;
5) and (3) precipitation: concentrating the liquid subjected to ion exchange in the step 4) by 3.8-4.5 times by using an evaporator to obtain concentrated solution, wherein the evaporation temperature is 70-88 ℃; precipitating with 70-80% ethanol at a volume ratio of the concentrated solution to ethanol of 1:2.6 (V/V);
6) solid-liquid separation is carried out on the precipitate obtained in the step 5), the separated solid is added with 75-80% ethanol for the first time, and the content of the suspended solid is 1.5% (V/V); solid-liquid separation, adding 80-88% ethanol into the separated solid matter, and cleaning for the second time, wherein the content of the suspended solid matter is 1.5% (V/V);
7) cleaning, press filtering to obtain pectin solid with dry matter content greater than 45%, spraying 5% sodium carbonate aqueous solution to adjust pectin pH to more than 3.0, drying until water content is less than 10%, and drying at 85-95 deg.C for 1.5-2.5 hr with boiling drier; pulverizing to 60-80 mesh.
Example 4
A method for producing pectin by blending dry and wet raw materials comprises the following steps:
1) weighing dried raw materials (dried lemon peels), adding water, performing ultrasonic cleaning for 15-30min, wherein the material-liquid ratio by mass is 1:20(W/W), performing solid-liquid separation, and then putting into an extraction tank for extraction, wherein an extracting solution is nitric acid water with the pH value of 2.3 (adjusted to the pH value of 2.3 by using 65-68% nitric acid), the material-liquid ratio is 1:40, and the extraction is performed for 1-1.5 hours;
2) simultaneously, preparing wet raw materials (wet lemon peels after juicing), crushing to 1-3mm, weighing, adding water, and performing ultrasonic cleaning for 15-30min, wherein the material-liquid ratio by mass in cleaning is 1: 8(W/W), performing solid-liquid separation, squeezing to the water content of less than 75%, and repeating the washing once.
3) After the dry raw materials are subjected to extraction reaction for 1-1.5 hours, adding the wet raw materials prepared in the step 2) until the material-liquid ratio is 1:6, adding 65-68% nitric acid to adjust the pH value to 2.3, and continuously performing extraction reaction for 4 hours; adding 22-25% ammonia water to adjust pH to 2.8-3.2 to terminate the reaction; separating solid and liquid to obtain primary extractive solution, coarse filtering with plate and frame filter press, and fine filtering with leaf filter.
4) Performing ion exchange on the primary extractive solution with 711 cation exchange resin at pH2.8-3.2 of 30% and 60-75 deg.C for 120 min;
5) and (3) precipitation: concentrating the liquid subjected to ion exchange in the step 4) by 3.8-4.5 times by using an evaporator to obtain concentrated solution, wherein the evaporation temperature is 70-88 ℃; precipitating with 70-80% ethanol at a volume ratio of concentrated solution to ethanol of 1:2-1:2.6 (V/V);
6) solid-liquid separation is carried out on the precipitate obtained in the step 5), the separated solid is added with 75-80% ethanol for the first time, and the content of the suspended solid is 0.7-2.5% (V/V); solid-liquid separation, adding 80-88% ethanol into the separated solid matter for secondary cleaning, wherein the content of the suspended solid matter is 0.5-2.2% (V/V);
7) cleaning, press filtering to obtain pectin solid with dry matter content greater than 45%, spraying 5% sodium carbonate aqueous solution to adjust pectin pH to more than 3.0, drying until water content is less than 10%, and drying at 85-95 deg.C for 1.5-2.5 hr with boiling drier; pulverizing to 60-80 mesh.
Example 5
The pectins prepared in examples 1 to 4 were tested and their performance parameters are shown in Table 1.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (9)
1. A production method of dry and wet raw material blended pectin is characterized by comprising the following steps:
1) adding water into dried lemon peel, performing ultrasonic cleaning at a material-liquid ratio of 1:10-20(W/W), performing solid-liquid separation, and extracting with nitric acid water at pH of 1.0-2.8 at an extraction material-liquid ratio of 1:20-40 for 1-1.5 hr;
2) the method comprises the following steps of crushing wet lemon peels, adding water for ultrasonic cleaning, wherein the material-liquid ratio by mass in cleaning is 1:3-8 (W/W), performing solid-liquid separation, squeezing until the water content is less than 75%, and repeating the cleaning once;
3) after the extraction reaction of the dried lemon peel is carried out for 1 to 1.5 hours, adding the prepared wet raw material in the step 2) until the material-liquid ratio is 1:3-8, adding nitric acid to adjust the pH value to be 1.0 to 2.8, and continuing the extraction reaction for 2 to 4 hours; then adding ammonia water to adjust the pH value to 2.8-3.2 to terminate the reaction; performing solid-liquid separation to obtain primary extract;
4) performing ion exchange on the primary extract with cation exchange resin at pH2.8-3.2 and pH 60-75% in an amount of 10-30% for 100-120 min.
2. The method for producing dry and wet raw material blended pectin according to claim 1, wherein the ultrasonic water cleaning feed-liquid ratio in step 1) is 1:10-12 (W/W).
3. The method for producing pectin by blending dry and wet raw materials according to claim 1, wherein the extracting solution in step 1) is nitric acid water with pH of 1.1-2.4, and the ratio of the material to the liquid is 1: 20-30.
4. The method for producing dry and wet raw material blended pectin according to claim 1, wherein the ratio of cleaning solution to cleaning solution in step 2) is 1: 3-4(W/W), adding nitric acid to adjust the pH value to 1.1-2.4.
5. The method for producing pectin by blending dry and wet raw materials according to claim 1, wherein the solid-liquid separation in step 3) is performed by coarse filtration using a plate and frame filter press and fine filtration using a leaf filter.
6. The method for producing dry and wet raw material blended pectin according to claim 1, wherein the amount of the cation exchange resin in step 4) is 15-25%.
7. The method for producing pectin by blending dry and wet raw materials according to any of claims 1 to 6, wherein the method for producing pectin further comprises the step of 5) precipitating: concentrating the liquid subjected to ion exchange in the step 4) by 3.8-4.5 times by using an evaporator to obtain concentrated solution, wherein the evaporation temperature is 70-88 ℃; precipitating with 70-80% ethanol at a volume ratio of concentrated solution to ethanol of 1:2-1:2.6 (V/V).
8. The method for producing pectin by blending dry and wet raw materials according to claim 7, wherein the method for producing pectin further comprises the step 6): performing solid-liquid separation on the precipitate obtained in the step 5), adding 75-80% ethanol into the separated solid matter, and cleaning for the first time, wherein the content of the suspended solid matter is 0.7-2.5% (V/V); solid-liquid separation, adding 80-88% ethanol into the separated solid matter for secondary cleaning, wherein the content of the suspended solid matter is 0.5-2.2% (V/V); and (4) performing solid-liquid separation and drying.
9. The method for producing pectin by blending dry and wet raw materials according to claim 8, wherein the solid-liquid separation and drying is washing and then press-filtering to obtain pectin solids with dry matter content of more than 45%, spraying 5% sodium carbonate aqueous solution to adjust pH of pectin to be more than 3.0,
finally drying until the water content is less than 10%, and drying for 1.5-2.5h at 85-95 ℃ by using a boiling dryer; pulverizing to 60-80 mesh.
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| CN114617269A (en) * | 2022-03-24 | 2022-06-14 | 重庆檬泰生物科技有限公司 | Instant pectin and prebiotics compound production process |
| CN114634655A (en) * | 2022-03-24 | 2022-06-17 | 重庆檬泰生物科技有限公司 | Pectin production process for coating probiotics |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114617269A (en) * | 2022-03-24 | 2022-06-14 | 重庆檬泰生物科技有限公司 | Instant pectin and prebiotics compound production process |
| CN114634655A (en) * | 2022-03-24 | 2022-06-17 | 重庆檬泰生物科技有限公司 | Pectin production process for coating probiotics |
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