CN106883312A - A kind of extracting method of silkworm excrement pectin - Google Patents

A kind of extracting method of silkworm excrement pectin Download PDF

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Publication number
CN106883312A
CN106883312A CN201510935454.2A CN201510935454A CN106883312A CN 106883312 A CN106883312 A CN 106883312A CN 201510935454 A CN201510935454 A CN 201510935454A CN 106883312 A CN106883312 A CN 106883312A
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Prior art keywords
silkworm excrement
pectin
extracting method
take
silkworm
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宁发子
万雪峰
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Dou Hao Bio Tech Ltd Chongqing
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Dou Hao Bio Tech Ltd Chongqing
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    • CCHEMISTRY; METALLURGY
    • 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

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Molecular Biology (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention discloses a kind of method of silkworm excrement pectin extraction pectin, described method is that raw material passes through the steps such as enzymolysis and ultrasonically treated, decolouring, vacuum freeze drying to extract the removing green silkworm excrement after chlorophyll.The beneficial effects of the invention are as follows, by complex enzyme and ultrasonic wave collective effect in silkworm excrement, pectin, enzyme effect mild condition are extracted from silkworm excrement, and also act as the effect of broken wall, make the effect of pectin in silkworm excrement thoroughly dissolution;Ultrasonic wave extraction process is a physical process, without chemical change in extraction process, recovery rate it is high and it is effective protection extract functional component.The inventive method solves the problems, such as that the silkworm excrement waste material of chlorophyll factory, without place stacking, furthermore achieved that the comprehensive utilization of silkworm excrement, improves the economic worth of silkworm excrement.

Description

A kind of extracting method of silkworm excrement pectin
Technical field
Biological technical field of the present invention, and in particular to be a kind of extracting method of silkworm excrement pectin.
Background technology
Pectin as food additives, can be widely used for food industry abandoned as thickener village gelling, stabilizer, emulsifying agent etc..Pectin is primarily present in the plant stem-leaf body such as vegetables and fruit, plays the role of to remove heavy metal to human body.Sericulture is traditional cause of China, and enormous amount, silkworm is food with mulberry leaf, and the excrement of silkworm is to contain multiple beneficial composition in silkworm excrement, such as chlorophyll pectin, according to incompletely statistics, there is nearly ten million ton of silkworm excrement in China every year, and resource is quite enriched, comprehensive development and utilization silkworm excrement has economic worth very high current, in addition to having and being used to extract chlorophyll on a small quantity, all as Fertilizer application, its economic worth could not make full use of major part silkworm excrement.Pectin content is still at a relatively high during silkworm excrement extracts the residue after chlorophyll.
The content of the invention
The invention provides a kind of to extract the method that the removing green silkworm excrement after chlorophyll extracts silkworm excrement pectin as raw material.
The present invention uses following technical scheme:
A kind of extracting method of silkworm excrement pectin, comprises the following steps:
(1) it is beaten, digest, filters:Press silkworm excrement and water (g/ml) 1:The ratio of 4-8 adds water, and silkworm excrement is beaten into 3-5min with beater, adjusts its temperature to 35-55 DEG C, and pH to 5.5-6.5 adds cellulase, the complex enzyme of acid protease composition, digests 2h, obtains enzymolysis liquid;
(2)It is ultrasonically treated:It is 1.0-1.5 to take enzymolysis liquid inorganic acid and adjust PH, is warming up to 80-90 DEG C, ultrasonication 70-80min under the power of 175W;Filtrate to be filtered to take with 800-1000 mesh filter screens standby again;
(3)Decolourize:To step(2)Activated carbon decolorizing is added in gained filtrate, activated carbon is 1g with the mass volume ratio of solution:100rpm treatment 30-40min under the conditions of 100-150mL, 70-80 DEG C, filtering, filtrate decompression is concentrated into the 1/5 of original volume;
(4)Dry:Take step(3)Obtained concentrate, adds 0.5~1.5 times of 95% ethanol of weight, stands 10~30 minutes, and suction filtration, precipitation is washed several times with 75% ethanol, and centrifugation, the sediment that will be centrifugally separating to obtain is dried under the conditions of 50~60 DEG C, i.e. finished product.
Preferably, step(2)Described in cellulase, the part by weight of acid protease be:1-4 :1;The gross weight of described complex enzyme accounts for the 1-3% of silkworm excrement;
It is further preferred that step(2)In, the inorganic acid is hydrochloric acid.
Still more preferably, step(3)In, the temperature concentrated under reduced pressure is 70~75 DEG C.
Beneficial effects of the present invention are:
(1)By complex enzyme and ultrasonic wave collective effect in raw material, pectin, enzyme effect mild condition are extracted from raw material, and also act as the effect of broken wall, make the effect of pectin in raw material thoroughly dissolution;Ultrasonic wave extraction process is a physical process, and without chemical change in extraction process, the bioactivator being leached keeps constant in a short time, shortens the broken time;
(2)Judder, acceleration high, stirring action produced using ultrasonic wave etc. can accelerate the dissolution of effective ingredients in plant, so as to improve recovery rate, save solvent.
(3)Joint is taken short using pectin in enzymolysis and ultrasonically treated extraction silkworm excrement;The extracting factor such as ultrasonic power, extraction time, extractant and its concentration, solid-liquid ratio takes optimal, recovery rate it is high and it is effective protection extract functional component.
Specific embodiment
It is described further with embodiment below, but the present invention is not limited to these embodiments.
Embodiment 1
A kind of extracting method of silkworm excrement pectin, step is as follows:
(1) it is beaten, digest, filters:Silkworm excrement 100g is taken, the pure water of 400ml is added, silkworm excrement is beaten 3min with beater, adjust its temperature to 35 DEG C, pH to 5.5 adds 1 g by cellulase, acid protease(1:1)The complex enzyme of composition, digests 2h, obtains enzymolysis liquid;
(2)It is ultrasonically treated:It is 1.00 to take enzymolysis liquid hydrochloric acid and adjust PH, is warming up to 80 DEG C, ultrasonication 80min under the power of 175W;Supernatant to be filtered to take with 800-1000 mesh filter screens standby again;
(3)Decolourize:To step(2)Activated carbon decolorizing is added in gained ultrasonication solution, activated carbon is 1g with the mass volume ratio of solution:100mL, 100rpm treatment 30min under the conditions of 70 DEG C, filtering, filtrate is concentrated under reduced pressure into the 1/5 of original volume at 70~75 DEG C;
(4)Dry:Take step(3)Obtained concentrate, adds 0.5 times of 95% ethanol of weight, stands 30 minutes, suction filtration, precipitation is washed several times with 75% ethanol, centrifugation, the sediment that will be centrifugally separating to obtain is dried under the conditions of 50 DEG C, obtains final product pectin finished product 13.65g, and product yield is 13.65%.
Example 2
A kind of extracting method of silkworm excrement pectin, step is as follows:
(1)Mashing, enzymolysis, filtering:The pure water that silkworm excrement 100g adds 800ml is taken, its temperature to 55 DEG C is adjusted, pH to 6.5 adds 3g by cellulase, acid protease(4:1)The complex enzyme of composition, digests 2h, obtains enzymolysis liquid;
(2)It is ultrasonically treated:It is 1.50 to take enzymolysis liquid hydrochloric acid and adjust PH, is warming up to 90 DEG C, ultrasonication 70min under the power of 175W;Supernatant to be filtered to take with 800-1000 mesh filter screens standby again;
(3)Decolourize:To step(2)Activated carbon decolorizing is added in gained ultrasonication solution, activated carbon is 1g with the mass volume ratio of solution:150mL, 100rpm treatment 40min under the conditions of 70 DEG C, filtering, filtrate is concentrated under reduced pressure into the 1/5 of original volume at 70~75 DEG C;
(4)Dry:Take step(3)Obtained concentrate, adds 1.5 times of 95% ethanol of weight, stands 10 minutes, suction filtration, precipitation is washed several times with 75% ethanol, centrifugation, the sediment that will be centrifugally separating to obtain is dried under the conditions of 60 DEG C, obtains final product pectin finished product 13.43g, and product yield is 13.43%.
Embodiment 3
A kind of extracting method of silkworm excrement pectin, step is as follows:
(1)Mashing, enzymolysis, filtering:The pure water that silkworm excrement 100g adds 600ml is taken, silkworm excrement is beaten 4min with beater, adjust its temperature to 45 DEG C, pH to 6.0 adds 2g by cellulase, acid protease(2.5:1)The complex enzyme of composition, digests 2h, obtains enzymolysis liquid;
(2)It is ultrasonically treated:It is 1.25 to take enzymolysis liquid hydrochloric acid and adjust PH, is warming up to 85 DEG C, ultrasonication 75min under the power of 175W;Supernatant to be filtered to take with 800-1000 mesh filter screens standby again;
(3)Decolourize:To step(2)Activated carbon decolorizing is added in gained ultrasonication solution, activated carbon is 1g with the mass volume ratio of solution:125mL, 100rpm treatment 40min under the conditions of 70 DEG C, filtering, filtrate is concentrated under reduced pressure into the 1/5 of original volume at 70~75 DEG C;
(4)Dry:Take step(3)Obtained concentrate, adds 1 times of 95% ethanol of weight, stands 20 minutes, suction filtration, precipitation is washed several times with 75% ethanol, centrifugation, the sediment that will be centrifugally separating to obtain is dried under the conditions of 55 DEG C, obtains final product pectin finished product 13.68g, and product yield is 13.68%.

Claims (4)

1. a kind of extracting method of silkworm excrement pectin, it is characterised in that comprise the following steps:
(1) it is beaten, digest, filters:Press silkworm excrement and water (g/ml) 1:The ratio of 4-8 adds water, and silkworm excrement is beaten into 3-5min with beater, adjusts its temperature to 35-55 DEG C, and pH to 5.5-6.5 adds cellulase, the complex enzyme of acid protease composition, digests 2h, obtains enzymolysis liquid;
(2)It is ultrasonically treated:It is 1.00-1.5 to take enzymolysis liquid inorganic acid and adjust PH, is warming up to 80-90 DEG C, 175W Power under ultrasonication 70-80min;Filtrate to be filtered to take with 800-1000 mesh filter screens standby again;
(3)Decolourize:To step(2)Activated carbon decolorizing is added in gained filtrate, activated carbon is 1g with the mass volume ratio of solution:100rpm treatment 30-40min under the conditions of 100-150mL, 70-80 DEG C, filtering, filtrate decompression is concentrated into the 1/5 of original volume;
(4)Dry:Take step(3)Obtained concentrate, adds 0.5~1.5 times of 95% ethanol of weight, stands 10~30 minutes, and suction filtration, precipitation is washed several times with 75% ethanol, and centrifugation, the sediment that will be centrifugally separating to obtain is dried under the conditions of 50~60 DEG C, i.e. finished product.
2. the extracting method of a kind of silkworm excrement pectin according to claim 1, it is characterised in that:Step(2)In, described cellulase, the part by weight of acid protease are:1-4 :1;The gross weight of described complex enzyme accounts for the 1-3% of silkworm excrement.
3. the extracting method of a kind of silkworm excrement pectin according to claim 1, it is characterised in that:Step(2)In, the inorganic acid is hydrochloric acid.
4. the extracting method of a kind of silkworm excrement pectin according to claim 1, it is characterised in that:Step(3)In, the temperature concentrated under reduced pressure is 70~75 DEG C.
CN201510935454.2A 2015-12-15 2015-12-15 A kind of extracting method of silkworm excrement pectin Pending CN106883312A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107245114A (en) * 2017-08-04 2017-10-13 浙江理工大学 The extraction of pectin and its content assaying method in a kind of silkworm excrement
CN112062874A (en) * 2020-09-16 2020-12-11 安徽农业大学 Mulberry leaf gel and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107245114A (en) * 2017-08-04 2017-10-13 浙江理工大学 The extraction of pectin and its content assaying method in a kind of silkworm excrement
CN112062874A (en) * 2020-09-16 2020-12-11 安徽农业大学 Mulberry leaf gel and preparation method and application thereof

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