CN109306026A - The fractional extraction method of citrus pectin and application - Google Patents

The fractional extraction method of citrus pectin and application Download PDF

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CN109306026A
CN109306026A CN201810818024.6A CN201810818024A CN109306026A CN 109306026 A CN109306026 A CN 109306026A CN 201810818024 A CN201810818024 A CN 201810818024A CN 109306026 A CN109306026 A CN 109306026A
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extraction method
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CN109306026B (en
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齐军茹
黄莹星
廖劲松
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Jiangxi Laimeng Biotechnology Co.,Ltd.
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South China University of Technology SCUT
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0045Homoglycans, 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
    • C08B37/0048Processes of extraction from organic materials
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/12Fermented milk preparations; Treatment using microorganisms or enzymes
    • A23C9/13Fermented milk preparations; Treatment using microorganisms or enzymes using additives
    • A23C9/1307Milk products or derivatives; Fruit or vegetable juices; Sugars, sugar alcohols, sweeteners; Oligosaccharides; Organic acids or salts thereof or acidifying agents; Flavours, dyes or pigments; Inert or aerosol gases; Carbonation methods
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/12Fermented milk preparations; Treatment using microorganisms or enzymes
    • A23C9/13Fermented milk preparations; Treatment using microorganisms or enzymes using additives
    • A23C9/137Thickening substances
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/152Milk preparations; Milk powder or milk powder preparations containing additives
    • A23C9/154Milk preparations; Milk powder or milk powder preparations containing additives containing thickening substances, eggs or cereal preparations; Milk gels
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/152Milk preparations; Milk powder or milk powder preparations containing additives
    • A23C9/156Flavoured milk preparations ; Addition of fruits, vegetables, sugars, sugar alcohols or sweeteners
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L21/00Marmalades, jams, jellies or the like; Products from apiculture; Preparation or treatment thereof
    • A23L21/10Marmalades; Jams; Jellies; Other similar fruit or vegetable compositions; Simulated fruit products
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/231Pectin; Derivatives thereof
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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Abstract

The invention belongs to food additives field, fractional extraction method and the application of a kind of citrus pectin are disclosed.Orange peel is added to the water after drying mixing, and adding acid for adjusting pH value is that 1.8~2.2,65~75 DEG C of stirrings are extracted, and centrifugation obtains level-one pectin extracting soln and level-one pectin slag;Level-one pectin slag is added to the water, adding acid for adjusting pH value is that 1.5~1.7,75~85 DEG C of stirrings are extracted, and centrifugation obtains second level pectin extracting soln and waste residue;Level-one pectin extracting soln and second level pectin extracting soln are rotated to the ethanol solution alcohol precipitation after 0.5~2.0h with 1~2 times of volume under the conditions of 55~65 DEG C, washed, it is dry, respectively obtain level-one pectin and second level pectin.The present invention realizes the grading extraction of pectin, solves the problems, such as that current pectin extraction is insufficient, and realize the classification of pectin finished product, realizes the rank diversification of pectin product.

Description

The fractional extraction method of citrus pectin and application
Technical field
The invention belongs to food additives fields, and in particular to a kind of fractional extraction method of citrus pectin and application.
Background technique
Citrus is the types of fruits of world wide production first, yield more than 100,000,000 tons, account for world's fruit sum five/ One, year the volume of trade occupy third in international trade agricultural product.40% or so of world's orange yield be used to process, and citrus adds Work waste material accounts for about the 50% of fruit weight based on pericarp, pulp slag and seed, containing many utilities, such as pectin, class Flavones, essential oil and pigment etc..Available substance rich in, the especially content of pectin, can reach dry in orange peel The 20%~30% of matter, the 70% of commodity pectin is extracted from orange peel in the world, is industrial metaplasia domestic and international at present Produce the main source of pectin.Orange peel is to be rich in the raw material for extracting pectin value, along with flourishing for citrus industry, citrus The processing of skin slag is increasingly becoming Citrus procession enterprise and realizes raw material using the bottleneck problem optimized.Optimize orange peel and extracts pectin Process conditions, will to Citrus procession research and innovation and improve Citrus procession productivity effect be of great significance.
It is also weaker for the industrialization of orange peel extraction pectin so far.Pectin is that a kind of natural solubility is more Sugar has the function of good physiological function and physics and chemistry, is a kind of food ingredient of nutrient health, is answered extensively in the food industry With.Pectin is widely used in jelly, jam, candy, acidic dairy prod and fruit juice etc. frequently as stabilizer, gelling agent and thickener In food, also because its is biodegradable and bio-compatible, it is applied to the industries such as medicine, weaving, printing and dyeing and cosmetics.
Currently, the technique that China extracts pectin is confined to once extract mostly, in fact, by the orange peel once extracted Slag also remains a large amount of pectin, and pectin extraction is simultaneously insufficient, and the most color of pectin produced is deep, poor quality.
Summary of the invention
In place of the above shortcoming and defect of the existing technology, the primary purpose of the present invention is that providing a kind of citrus The fractional extraction method of class pectin.The method of the present invention carries out grading extraction, available different stage, different qualities to orange peel And the pectin in different application field, and at the same time strict control extraction conditions, improve pectin yield.
Another object of the present invention is to provide a kind of pectin being prepared by the above method.
A further object of the present invention is to provide the applications of the pectin obtained using above method grading extraction.
The object of the invention is achieved through the following technical solutions:
A kind of fractional extraction method of citrus pectin, the specific steps are as follows:
Then plus acid for adjusting pH value (1) orange peel is added to the water after drying, is stirred at a temperature of 25~35 DEG C, It stirs and extracts at a temperature of being 1.8~2.2,65~75 DEG C, centrifugation obtains level-one pectin extracting soln and level-one pectin slag;
(2) level-one pectin slag obtained by step (1) is added to the water, adding acid for adjusting pH value is 1.5~1.7,75~85 DEG C At a temperature of stir extract, centrifugation, obtain second level pectin extracting soln and waste residue;
(3) level-one pectin extracting soln and second level pectin extracting soln are rotated into 0.5~2.0h under the conditions of 55~65 DEG C Afterwards with the ethanol solution alcohol precipitation of 1~2 times of volume, wash, it is dry, respectively obtain level-one pectin and second level pectin.
Preferably, drying described in step (1) refers to forced air drying or freeze-drying.
Preferably, the orange peel after dry in step (1) is mixed with water by 1:(20~30) material-water ratio;When being stirred Between be 0.5~1.0h.
Preferably, acid described in step (1) and step (2) refers in the nitric acid, hydrochloric acid, oxalic acid of 0.1~1mol/L It is at least one.
Preferably, the time that extraction is stirred described in step (1) is 1.5~2.5h.
Preferably, the time that extraction is stirred described in step (2) is 1.0~1.5h.
Preferably, the ethanol water that ethanol solution described in step (3) refers to dehydrated alcohol or volume fraction is 95%.
Preferably, alcohol precipitation described in step (3), which refers to, is added to pectin solution in ethanol solution, staticly settles.
Preferably, centrifugation described in step (1) and step (2) refer under the conditions of 6000~8000rpm centrifugation 20~ 30min。
A kind of level-one pectin and second level pectin, are prepared by the above method.
Application of the level-one pectin that the above method is prepared in acidic milk drink, second level pectin is in jam product Using.
Compared with the existing technology, extracting method of the invention and obtained product have the following advantages that and the utility model has the advantages that
(1) present invention is optimized final product quality, is greatlyd improve by control Extracting temperature, extraction time, alcohol precipitation condition The utilization rate of raw material, improves the production efficiency of pectin;
(2) present invention realizes the grading extraction of pectin, solves the problems, such as that current pectin extraction is insufficient, and realize The rank diversification of pectin product is realized in the classification of pectin finished product;
(3) present invention is prepared for level-one pectin, second level pectin, and level-one pectin is mainly used in acidic milk drink, second level fruit Glue is mainly used in jam product, realizes that pectin product applies upper Focus;
(4) grading extraction pectin method of the present invention has wide range of applications, and can be used for orange peel, lemon peel, orange peel, apple The grading extraction of pectin in the pericarps such as skin, pomelo peel.
Detailed description of the invention
Fig. 1 is viscosity and rate of deposition of the Yogurt Drink of level-one pectin of the present invention preparation under condition of different pH Result figure.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited In this.
Embodiment 1
(1) the orange peel 40g dried is soaked in 800mL deionized water, the stirring in water bath 0.5h under the conditions of 30 DEG C, with grass Acid solution adjusts pH to 1.8, the stirring in water bath 1.5h under the conditions of 70 DEG C.Level-one pectin extracting soln and level-one pectin are obtained after centrifugation Slag.
(2) level-one pectin slag is added into 450mL deionized water, adjusts pH to 1.7, the water-bath under the conditions of 80 DEG C with oxalic acid solution Stir 1h.Second level pectin extracting soln and waste residue are obtained after centrifugation.
(3) level-one pectin extracting soln and second level pectin extracting soln are rotated into 0.5h under the conditions of 65 DEG C, according to first plus The sequence to feed intake after alcohol carries out alcohol precipitation with 95% ethanol solution of 1.5 times of volumes, and washs, after dried under the conditions of 60 DEG C, obtain To level-one pectin 7.688g, second level pectin 3.196g, obtained pectin gross weight is 10.884g, and level-one pectin viscosity is 104.50mPas, second level pectin viscosity are 74.83mPas.
Embodiment 2
(1) the orange peel 40g of forced air drying is soaked in 1000mL deionized water, the stirring in water bath under the conditions of 35 DEG C 1.0h adjusts pH to 2.0, the water-bath 2.0h under the conditions of 65 DEG C with hydrochloric acid solution.Level-one pectin extracting soln and one are obtained after centrifugation Grade pectin slag.
(2) level-one pectin slag is added into 450mL deionized water, adjusts pH to 1.6, the water-bath under the conditions of 75 DEG C with hydrochloric acid solution Stir 1.5h.Second level pectin extracting soln and waste residue are obtained after centrifugation.
(3) after level-one pectin extracting soln and second level pectin extracting soln being rotated 1.0h under the conditions of 60 DEG C, according to elder generation Add the sequence to feed intake after alcohol, carry out alcohol precipitation with the dehydrated alcohol of equal volume, and wash, after dried under the conditions of 60 DEG C, obtain Level-one pectin 7.279g, second level pectin 3.074g, obtained pectin gross weight are 10.353g, and level-one pectin viscosity is 90.17mPas, second level pectin viscosity are 70.50mPas.
Embodiment 3
(1) the orange peel 30g being freeze-dried is soaked in 900mL deionized water, the stirring in water bath 0.5h under the conditions of 30 DEG C, PH to 2.2, the water-bath 2.0h under the conditions of 75 DEG C are adjusted with nitric acid solution.Level-one pectin extracting soln and level-one pectin are obtained after centrifugation Slag.
(2) level-one pectin slag is added into 450mL deionized water, adjusts pH to 1.5, the water-bath under the conditions of 80 DEG C with oxalic acid solution 1h.Second level pectin extracting soln and waste residue are obtained after centrifugation.
(3) level-one pectin extracting soln and second level pectin extracting soln are rotated into 1.5h under the conditions of 55 DEG C, after, according to elder generation After feeding intake plus alcohol sequence, carry out alcohol precipitation with 95% ethanol solution of two volumes, and wash, after dried under the conditions of 60 DEG C, Level-one pectin 7.036g, second level pectin 2.832g are obtained, obtained pectin gross weight is 9.868g, and level-one pectin viscosity is 91.20mPas, second level pectin viscosity are 72.75mPas.
Embodiment 4
(1) the lemon peel 40g of forced air drying is soaked in 800mL deionized water, the stirring in water bath under the conditions of 30 DEG C 0.5h adjusts pH to 2.0, the water-bath 2.5h under the conditions of 70 DEG C with nitric acid solution.Level-one pectin extracting soln and one are obtained after centrifugation Grade pectin slag.
(2) level-one pectin slag is added into 450mL deionized water, adjusts pH to 1.6, the water-bath under the conditions of 80 DEG C with oxalic acid solution 1h.Second level pectin extracting soln and waste residue are obtained after centrifugation.
(3) after level-one pectin extracting soln and second level pectin extracting soln being rotated 0.5h under the conditions of 60 DEG C, according to elder generation Add the sequence to feed intake after alcohol, carry out alcohol precipitation with the dehydrated alcohol of two volumes, and wash, after dried under the conditions of 60 DEG C, obtain Level-one pectin 4.336g, second level pectin 3.117g, obtained pectin gross weight are 7.453g, and level-one pectin viscosity is 86.33mPa S, second level pectin viscosity are 28.67mPas.
Embodiment 5
(1) the orange peel 40g being freeze-dried is soaked in 1000mL deionized water, the stirring in water bath under the conditions of 35 DEG C 1.0h adjusts pH to 1.9, the water-bath 1.5h under the conditions of 75 DEG C with hydrochloric acid solution.Level-one pectin extracting soln and one are obtained after centrifugation Grade pectin slag.
(2) level-one pectin slag is added into 450mL deionized water, adjusts pH to 1.6, the water-bath under the conditions of 80 DEG C with oxalic acid solution 1.5h.Second level pectin extracting soln and waste residue are obtained after centrifugation.
(3) after level-one pectin extracting soln and second level pectin extracting soln being rotated 2.0h under the conditions of 55 DEG C, according to elder generation Add the sequence to feed intake after alcohol, carry out alcohol precipitation with the dehydrated alcohol of 1.5 times of volumes, and wash, after dried under the conditions of 60 DEG C, obtain Level-one pectin 6.644g, second level pectin 1.384g, obtained pectin gross weight are 8.028g, and level-one pectin viscosity is 72.67mPa S, second level pectin viscosity are 37.67mPas.
The application experiment of gained level-one pectin of the invention, the preparation of Yogurt Drink:
The skimmed milk powder for weighing certain mass, is dissolved in deionized water, and 35~40 DEG C of stirring in water bath dissolutions 30~ 40min.It is warming up to 90~95 DEG C of heat preservation 10min sterilizings.Solution is taken out, is cooled to 40~45 DEG C, inoculation, ferment 8~12h.Hair After ferment under the conditions of 4 DEG C 10~14h of after-ripening.It weighs a certain amount of level-one pectin and white granulated sugar is dissolved in deionized water, 60 DEG C It is cooling stand-by after stirring in water bath dissolves 2h.Solidification cream after taking after-ripening is mixed with pectin solution, so that level-one pectin is in fermented type Additive amount in acidic milk drink is 3 ‰~6 ‰, is stirred evenly, and adjusts pH value of solution with citrate buffer solution, homogeneous is sent out Ferment type acidic milk drink.When pH is respectively 3.4~4.2, the viscosity and rate of deposition result of gained Yogurt Drink are such as Shown in Fig. 1.As seen from Figure 1, when pH is 3.8~4.0, resulting Yogurt Drink viscosity is 7.59~7.78mPa S, rate of deposition are 2.72~2.75 μm, and lotion is uniform, and quality is more stable.
The application experiment of gained second level pectin of the invention, the preparation of strawberry jam:
Strawberry is cleaned, color protection, is beaten after the pretreatment such as softening, while by a certain amount of white granulated sugar at 60~65 DEG C Under conditions of heat while stirring to being dissolved in pre-boiled liquid.Syrup is uniformly mixed with strawberry slurry, 3 ‰ second level fruit is added Glue, after with citric acid tune pH value be 3.3~3.7, be concentrated under the conditions of 70~80 DEG C, concentration time control for 20~ 30min.Under this condition, the strawberry jam solid content obtained is 35%~40%, gel strength 7.10g, and gel is uniform And the sauce body retentiveness of jam is preferable.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention, It should be equivalent substitute mode, be included within the scope of the present invention.

Claims (10)

1. a kind of fractional extraction method of citrus pectin, it is characterised in that specific step is as follows:
(1) orange peel is added to the water after drying, is stirred at a temperature of 25~35 DEG C, then plus acid for adjusting pH value is It stirs and extracts at a temperature of 1.8~2.2,65~75 DEG C, centrifugation obtains level-one pectin extracting soln and level-one pectin slag;
(2) level-one pectin slag obtained by step (1) is added to the water, adding acid for adjusting pH value is 1.5~1.7,75~85 DEG C of temperature Lower stirring is extracted, and centrifugation obtains second level pectin extracting soln and waste residue;
(3) level-one pectin extracting soln and second level pectin extracting soln are rotated under the conditions of 55~65 DEG C after 0.5~2.0h with 1 The ethanol solution alcohol precipitation of~2 times of volumes washs, dry, respectively obtains level-one pectin and second level pectin.
2. a kind of fractional extraction method of citrus pectin according to claim 1, it is characterised in that: institute in step (1) It states drying and refers to forced air drying or freeze-drying.
3. a kind of fractional extraction method of citrus pectin according to claim 1, it is characterised in that: done in step (1) Orange peel after dry is mixed with water by 1:(20~30) material-water ratio;Being stirred the time is 0.5~1.0h.
4. a kind of fractional extraction method of citrus pectin according to claim 1, it is characterised in that: step (1) and step Suddenly acid described in (2) refers at least one of nitric acid, hydrochloric acid, oxalic acid of 0.1~1mol/L.
5. a kind of fractional extraction method of citrus pectin according to claim 1, it is characterised in that: institute in step (1) Stating the time that stirring is extracted is 1.5~2.5h.
6. a kind of fractional extraction method of citrus pectin according to claim 1, it is characterised in that: institute in step (2) Stating the time that stirring is extracted is 1.0~1.5h.
7. a kind of fractional extraction method of citrus pectin according to claim 1, it is characterised in that: institute in step (3) State the ethanol water that ethanol solution refers to dehydrated alcohol or volume fraction is 95%;The alcohol precipitation, which refers to, adds pectin solution Enter into ethanol solution, staticly settles.
8. a kind of fractional extraction method of citrus pectin according to claim 1, it is characterised in that: step (1) and step Suddenly centrifugation described in (2) refers to 20~30min of centrifugation under the conditions of 6000~8000rpm.
9. a kind of level-one pectin and second level pectin, it is characterised in that: prepared by method according to any one of claims 1 to 8 It obtains.
10. application of the level-one pectin as claimed in claim 9 in acidic milk drink, second level pectin answering in jam product With.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112159485A (en) * 2019-09-20 2021-01-01 山东皇尊庄园山楂酒有限公司 Hawthorn pectin extraction process and hawthorn product
CN113501892A (en) * 2021-07-23 2021-10-15 江西莱檬生物科技有限责任公司 Combined extraction method for different functional components in citrus fruit peel residues
CN113647461A (en) * 2021-08-20 2021-11-16 成都市农林科学院 Double-protein yoghourt containing natto hormone and preparation method thereof
CN114712553A (en) * 2022-04-11 2022-07-08 浙江理工大学 Preparation method of wound dressing based on shaddock peel pectin-oxidized chitosan composite hydrogel

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JPS6176503A (en) * 1984-09-21 1986-04-19 Mitsubishi Acetate Co Ltd Purification of pectin
JPS6189204A (en) * 1984-10-08 1986-05-07 Mitsubishi Acetate Co Ltd Partial demethoxylation of pectin
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