CN109898096A - The method of citrus pectin oligosaccharide is prepared under the conditions of light current solution - Google Patents

The method of citrus pectin oligosaccharide is prepared under the conditions of light current solution Download PDF

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CN109898096A
CN109898096A CN201810520107.7A CN201810520107A CN109898096A CN 109898096 A CN109898096 A CN 109898096A CN 201810520107 A CN201810520107 A CN 201810520107A CN 109898096 A CN109898096 A CN 109898096A
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solution
pectin
added
electrolytic
conditions
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CN109898096B (en
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范传会
何建军
陈学玲
王少华
施建斌
梅新
隋勇
蔡沙
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Farm Product Processing and Nuclear Agricultural Technology Institute of Hubei Academy of Agricultural Sciences
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Farm Product Processing and Nuclear Agricultural Technology Institute of Hubei Academy of Agricultural Sciences
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Abstract

The present invention relates to a kind of methods that citrus pectin oligosaccharide is prepared under the conditions of light current solution, high ester citrus pectin is dissolved in sodium chloride solution, configure pectin solution, pectin solution is added to using graphite as in the electrolytic cell one of cathode, isoconcentration sodium chloride solution is added to platinum electrode as in the electrolytic cell two of anode;With the mode of DC electrolysis, it is electrolysed under the conditions of voltage 15~25V light current solution, is stirred respectively in electrolytic process;The electrolytic solution obtained in electrolytic cell one is collected, with hydrochloric acid by solution tune pH to 6~7;4 times of dehydrated alcohol precipitating is added;Precipitating is collected, dry is pectin oligosaccharide.Using the present invention, macromolecular high ester citrus pectin is electrolysed as small molecule pectin oligosaccharide under conditions of light current solution;It controls decomposition voltage and the time controls palliating degradation degree, to achieve the purpose that the POS for precisely preparing molecular weight 3000~8000, promote commodity value.It is low energy consumption of the present invention, environmental-friendly, it is easy to implement industrialized production.

Description

The method of citrus pectin oligosaccharide is prepared under the conditions of light current solution
Technical field
The present invention relates to the preparation methods of citrus pectin oligosaccharide, and in particular to one kind prepares citrus under the conditions of light current solution The method of pectin oligosaccharide.
Background technique
Oligosaccharide is the most common diet prebiotics, can by gastrointestinal bacterial flora ferment utilize, change microorganism composition and (or) activity, to promote host body healthy.Pectin oligosaccharide (pectic oligosaccharides, POS) is pectin warp The low molecular weight product oligosaccharides formed after depolymerisation are crossed, are a kind of novel prebiotics.POS usually passes through from agricultural wastes The preparation of the methods of physics, chemistry and biological enzyme is kept POS yield and purity lower, need to be carried out to POS due to material composition complexity Further separation and purifying, limit the application range of POS to a certain extent.Contain pectin oligosaccharide ingredient currently on the market Product is rare, price is high;Its main restricting factor is that POS technology of preparing is immature, cannot form large-scale production.It has registered POS preparation method (physical method, chemical method and biological enzyme etc.) there are pectin degrading is excessive or pectin degrading not exclusively, product The problems such as complicated component, high production cost, high energy consumption and environmental pollution, is not able to satisfy POS large scale preparation demand.
If CN105506029A discloses a kind of method for preparing antimycotic pectin oligosaccharide with orange peel, with pH4.5's Acetic acid-sodium acetate buffer mass concentration is the pectin solution of 1.0-1.1%, and pectase P21,40-50 DEG C of water-bath is added It is stirred to react, then enzyme deactivation is living in boiling water bath again, and obtained pectin oligosaccharide is mainly disaccharides and trisaccharide.CN106832049A is public A kind of pectin oligosaccharide acidolysis preparation method that molecular weight is 2000~3000Da has been opened, has first sent out citrus pectin and trifluoroacetic acid Raw reaction, is added ethanol precipitation into the supernatant after reaction, and precipitating drying is obtained.
Summary of the invention
The problems such as the purpose of the present invention is citrus POS technology of preparing is immature, classification is difficult, high energy consumption, provides a kind of essence The method of citrus pectin oligosaccharide is prepared under the conditions of the light current solution of quasi- control POS molecular weight.
The implementation of the object of the invention is the method that citrus pectin oligosaccharide is prepared under the conditions of light current solution, specific steps It is as follows:
1) 1g high ester citrus pectin is dissolved in the solution of 2% sodium chloride, is configured to 1% pectin solution, by pectin Solution is added in the electrolytic cell one using graphite as cathode, and the sodium chloride solution of isoconcentration is added to platinum electrode as just In the electrolytic cell two of pole;
2) it is electrolysed, is electrolysed by the way of DC electrolysis, 15~25V of voltage, 25 DEG C of electrolysis temperature, electrolysis time is 6~for 24 hours;Glass stirring rod agitating solution is used in electrolytic process respectively;
3) electrolytic solution in electrolytic cell one, obtained through step 2) is collected, and with hydrochloric acid by solution tune pH to 6~7;
4) dehydrated alcohol that 4 times of volumes are added through the electrolytic solution that step 3) obtains is precipitated;Precipitating is collected, precipitating is used 85% ethanol solution is washed till no chloride ion detection;Dry is pectin oligosaccharide.
The present invention uses the direct current of 15~25V, under conditions of light current solution, is by the electrolysis of macromolecular high ester citrus pectin The pectin oligosaccharide of small molecule;The palliating degradation degree of high ester citrus pectin is controlled by control decomposition voltage and electrolysis time, thus Achieve the purpose that precisely to prepare and be distributed in POS between 3000~8000, be advantageously implemented orientation depolymerized pectin, convenient for promoting citrus The commodity value of pectin POS.
It is low energy consumption of the present invention, environmental-friendly, it is easy to implement industrialized production.
Specific embodiment
High ester citrus pectin is dissolved in the solution of sodium chloride, achievement of allocation sol solution, by pectin solution be added to The sodium chloride solution of isoconcentration is added to the electrolytic cell two with platinum electrode as anode as in the electrolytic cell one of cathode by graphite It is interior;By the way of DC electrolysis, it is electrolysed under the conditions of voltage 15~25V light current solution, is stirred respectively in electrolytic process;It will electrolysis The electrolytic solution that obtains in slot one is collected, with hydrochloric acid by solution tune pH to 6~7;4 times of dehydrated alcohol precipitating is added;It is heavy to collect It forms sediment, dry is pectin oligosaccharide.
Pectin solution is added in the electrolytic cell one using graphite as cathode, the sodium chloride solution of isoconcentration is added to It is that pectin is added to electrolytic cell one because pectin shows negative point property as the reason in the electrolytic cell two of anode with platinum electrode Pectin is beneficial to prevent in electrolytic process in (near cathode) with the migration of electric current.Pectin its conductive energy as large biological molecule Power is weaker, the voltage that electrolyte sodium chloride is conducive to adjust electrolytic process is added, convenient for going on smoothly for electrolytic experiment.
Pectin used in the present invention is common high ester citrus pectin.
The present invention collects precipitating, dry, and drying means is heated-air drying, and drying condition is 6 hours at 40 DEG C.
The present invention is described in detail below with reference to example.
Embodiment 1
1) 1g high ester citrus pectin is dissolved in the solution of 2% sodium chloride, is configured to 1% pectin solution, by pectin Solution is added in the electrolytic cell one using graphite as cathode, and the sodium chloride solution of isoconcentration is added to platinum electrode as just In the electrolytic cell two of pole;
2) under the conditions of DC voltage 15V, 25 DEG C of temperature, it is electrolysed 6h;It is stirred respectively with glass stirring rod in electrolytic process Mix solution;
3) electrolytic solution in electrolytic cell one, obtained through step 2) is collected, and with hydrochloric acid by solution tune pH to 6~7;
4) dehydrated alcohol that 4 times of volumes are added through the electrolytic solution that step 3) obtains is precipitated;Precipitating is collected, precipitating is used 85% ethanol solution is washed till no chloride ion detection;
Using heated-air drying up to citrus POS.Drying condition is 6 hours dry at 40 DEG C.
Through to citrus POS carry out analysis learn, citrus POS molecular weight manufactured in the present embodiment between 4000~6000, Citrus POS yield is 30.43%.
Embodiment 2, with embodiment 1, unlike,
2) under the conditions of DC voltage 15V, 25 DEG C of temperature, it is electrolysed 12h;It is stirred respectively with glass stirring rod in electrolytic process Mix solution;
4) dehydrated alcohol that 4 times of volumes are added through the electrolytic solution that step 3) obtains is precipitated;Precipitating is collected, precipitating is used 85% ethanol solution is washed till no chloride ion detection;
Using heated-air drying up to citrus POS.Drying condition is 6 hours dry at 40 DEG C.
It is learnt through carrying out analysis to citrus POS,
For citrus POS molecular weight manufactured in the present embodiment between 4000~6000, citrus POS yield is 47.98%.
Embodiment 3, with embodiment 1, unlike,
2) under the conditions of DC voltage 15V, 25 DEG C of temperature, electrolysis is for 24 hours;It is stirred respectively with glass stirring rod in electrolytic process Mix solution;
4) dehydrated alcohol that 4 times of volumes are added through the electrolytic solution that step 3) obtains is precipitated;Precipitating is collected, precipitating is used 85% ethanol solution is washed till no chloride ion detection;
Using heated-air drying up to citrus POS.Drying condition is 6 hours dry at 40 DEG C.
Through to citrus POS carry out analysis learn, citrus POS molecular weight manufactured in the present embodiment between 4000~6000, Citrus POS yield is 64.51%.
Embodiment 4, with embodiment 1, unlike,
2) under the conditions of DC voltage 20V, 25 DEG C of temperature, it is electrolysed 6h;It is stirred respectively with glass stirring rod in electrolytic process Mix solution;
4) dehydrated alcohol that 4 times of volumes are added through the electrolytic solution that step 3) obtains is precipitated;Precipitating is collected, precipitating is used 85% ethanol solution is washed till no chloride ion detection;
Using heated-air drying up to citrus POS.Drying condition is 6 hours dry at 40 DEG C.Through analyzing citrus POS It learns, for citrus POS molecular weight manufactured in the present embodiment between 6000~8000, citrus POS yield is 44.67%.
Embodiment 5, with embodiment 1, unlike,
2) under the conditions of DC voltage 25V, 25 DEG C of temperature, it is electrolysed 12h;It is stirred respectively with glass stirring rod in electrolytic process Mix solution;
4) dehydrated alcohol that 4 times of volumes are added through the electrolytic solution that step 3) obtains is precipitated;Precipitating is collected, precipitating is used 85% ethanol solution is washed till no chloride ion detection;
Using heated-air drying up to citrus POS.Drying condition is 6 hours dry at 40 DEG C.
Through to citrus POS carry out analysis learn, citrus POS molecular weight manufactured in the present embodiment between 3000~5000, Citrus POS yield is 20.39%.

Claims (2)

1. preparing the method for citrus pectin oligosaccharide under the conditions of light current solution, it is characterised in that: specific step is as follows:
1) 1g high ester citrus pectin is dissolved in the solution of 2% sodium chloride, is configured to 1% pectin solution, by pectin solution It is added in the electrolytic cell one using graphite as cathode, the sodium chloride solution of isoconcentration is added to platinum electrode as anode In electrolytic cell two;
2) be electrolysed, be electrolysed using DC electrolysis by the way of, 15~25V of voltage, 25 DEG C of electrolysis temperature, electrolysis time for 6~ 24h;Glass stirring rod agitating solution is used in electrolytic process respectively;
3) electrolytic solution in electrolytic cell one, obtained through step 2) is collected, and with hydrochloric acid by solution tune pH to 6~7;
4) dehydrated alcohol that 4 times of volumes are added through the electrolytic solution that step 3) obtains is precipitated;Precipitating is collected, is precipitated with 85% Ethanol solution is washed till no chloride ion detection;Dry is pectin oligosaccharide.
2. preparing the method for citrus pectin oligosaccharide under the conditions of light current solution according to claim 1, it is characterised in that: step 4) heated-air drying is used, drying condition is 6 hours at 40 DEG C.
CN201810520107.7A 2018-05-28 2018-05-28 Method for preparing citrus pectin oligosaccharides under weak electrolysis condition Active CN109898096B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110387555A (en) * 2019-07-17 2019-10-29 湖北省农业科学院农产品加工与核农技术研究所 The method that light current solution prepares plant amylum glucan
CN116925257A (en) * 2023-07-20 2023-10-24 华南理工大学 Method for preparing low-methoxy orange peel pectin by regional temperature control and electrochemical cathode and anode co-operation

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102534650A (en) * 2012-01-18 2012-07-04 河北工业大学 Method for preparing glucose by electrochemically degrading fiber oligosaccharide
CN103820808A (en) * 2013-12-20 2014-05-28 广西科技大学 Degradation method of chitosan

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102534650A (en) * 2012-01-18 2012-07-04 河北工业大学 Method for preparing glucose by electrochemically degrading fiber oligosaccharide
CN103820808A (en) * 2013-12-20 2014-05-28 广西科技大学 Degradation method of chitosan

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110387555A (en) * 2019-07-17 2019-10-29 湖北省农业科学院农产品加工与核农技术研究所 The method that light current solution prepares plant amylum glucan
CN116925257A (en) * 2023-07-20 2023-10-24 华南理工大学 Method for preparing low-methoxy orange peel pectin by regional temperature control and electrochemical cathode and anode co-operation
CN116925257B (en) * 2023-07-20 2024-04-05 华南理工大学 Method for preparing low-methoxy orange peel pectin by regional temperature control and electrochemical cathode and anode co-operation

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