CN103739729B - A kind of Indigowoad root selenium polysaccharide and preparation method thereof - Google Patents

A kind of Indigowoad root selenium polysaccharide and preparation method thereof Download PDF

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CN103739729B
CN103739729B CN201310649081.3A CN201310649081A CN103739729B CN 103739729 B CN103739729 B CN 103739729B CN 201310649081 A CN201310649081 A CN 201310649081A CN 103739729 B CN103739729 B CN 103739729B
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polysaccharide
preparation
indigowoad root
selenium
banlangen
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CN103739729A (en
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陈小秋
何庆君
刘鼎阔
王立红
赵云英
赵晶晶
张俊霞
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Tianjin United Chuangyan Biomedical Technology Co ltd
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Dingzheng Animal Pharmaceutical Tianjin Co Ltd
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Abstract

The present invention relates to a kind of Indigowoad root selenium polysaccharide, Radix Isatidis and sodium chloride, water Hybrid Heating are extracted, then the Banlangen Polysaccharide of collection and selenizing agent are carried out catalytic reaction, last reactant is finished product. In the present invention, Indigowoad root selenium polysaccharide in finished product possesses the double effects of Banlangen Polysaccharide and organic selenium, the two be combined with each other, simultaneously act on body, the immunocompetence of body can be further enhanced, in clinical practice uses, it is to avoid poultry sudden deaths under scarce selenium and dysimmunity state, reduce the economic loss of raiser.

Description

A kind of Indigowoad root selenium polysaccharide and preparation method thereof
Technical field
The invention belongs to Banlangen Polysaccharide field of deep, especially a kind of Indigowoad root selenium polysaccharide and preparation method thereof.
Background technology
Radix Isatidis calls indigo-blue, Isatis indigotica Fort (Indigofera tinctoria L, Baphicanthus cusia (nees) Brem. Polygonum tinctorium Ait) root and Radix Clerodenri Cyrtophylli, is plant Isatis indigotica Fort. or the dry root of grass Folium Isatidis, and in elongated cylindrical, surface is light yellow, coarse, has vertical wrinkle and horizontal spot, and it is Chinese medicine, has the function of heat-clearing and toxic substances removing, removing heat from blood sore-throat relieving. For diseases such as maculae caused by virulent heat pathogen, crimson tongue purple dark, mumps, sore throat, scarlet fever, major part pestilence, erysipelas, carbuncle. In the numerous composition of Radix Isatidis, Banlangen Polysaccharide is one of main chemical composition, and research shows, it has immunoregulation capability, effect for reducing blood fat, antivirus action and effect of scavenging radical.
Organic selenium is that one follows Methionine metabolism approach metabolism, participate in the synthesis of albumen, easily store in tissue, absorb, if effect of Banlangen Polysaccharide and organic selenium can be combined with each other, will be formed and a kind of can play the organic selenium facilitation to body, the multifunctional product of Banlangen Polysaccharide effect can be embodied again.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that result of use is good, a kind of Indigowoad root selenium polysaccharide of being readily produced.
The present invention adopts the technical scheme that:
A kind of preparation method of Indigowoad root selenium polysaccharide, it is characterised in that: comprising the following steps: its raw material includes Banlangen Polysaccharide and selenizing agent, the weight ratio of the two is 1:0.2~0.85, and described selenizing agent is triphenyl selenizing phosphine, pyridine-dichloro oxygen selenium or sodium selenite;
(1) Banlangen Polysaccharide and selenizing agent are added in reactor jointly;
(2) reacting by heating still so that it is interior temperature rises to 40~65 degrees Celsius, the weight ratio adding catalyst lean nitric acid or barium chloride, catalyst and selenizing agent is 0.2~0.45:1, and the catalytic reaction time is 2~12 hours;
(3) centrifugation step product (2) under 500~1500 turns of conditions per minute, then adsorb with the macroporous resin in 100~500 nanometers of aperture;
(4) being washed by step macroporous resin (3) absolute ether, the product of eluting is centrifugal under 500~1500 turns of conditions per minute, and gleanings prepares finished product through dried;
The preparation method of described Banlangen Polysaccharide comprises the following steps:
1. jointly adding in Low Temperature Thermal reflux, extract, tank by Radix Isatidis and water, temperature is 70 degrees Celsius, and vacuum is 0.2 MPa;
2. add sodium chloride, then temperature in extraction pot is risen to 45~75 degrees Celsius and extract;
3. collect extracting solution, under 0.2~0.5 MPa of condition, carry out concentrating under reduced pressure, until relative density is 1.1~1.35 stoppings;
4. by step product 3. by detergent washing, then collected after centrifugation supernatant under 500~1500 turns of conditions per minute, then supernatant is prepared after 120 degrees Celsius of heated-air circulation oven inner dryings Banlangen Polysaccharide.
And, the weight ratio of step 1. described Radix Isatidis and water is 1:5~15.
And, addition is Radix Isatidis and water gross weight the 0.1~0.5% of step 2. described sodium chloride, extraction time is 2~8 hours.
And, step 4. described detergent is 95% ethanol or absolute ether, and the weight ratio between step product and detergent (3) is 1:3~5.
Advantages of the present invention and having the benefit effect that
In the present invention, Radix Isatidis and sodium chloride, water Hybrid Heating are extracted, then the Banlangen Polysaccharide of collection and selenizing agent being carried out catalytic reaction, last reactant is finished product, and the Indigowoad root selenium polysaccharide in finished product possesses the double effects of Banlangen Polysaccharide and organic selenium, the two be combined with each other, simultaneously act on body, the immunocompetence of body can be further enhanced, in clinical practice uses, avoid poultry sudden death under scarce selenium and dysimmunity state, reduce the economic loss of raiser.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, it is impossible to limits protection scope of the present invention with following embodiment.
A kind of Indigowoad root selenium polysaccharide, the innovation of the present invention is in that: its raw material includes Banlangen Polysaccharide and selenizing agent, and the weight ratio of the two is 1:0.2~0.85, and described selenizing agent is triphenyl selenizing phosphine, pyridine-dichloro oxygen selenium or sodium selenite.
The preparation method of above-mentioned Banlangen Polysaccharide comprises the following steps:
(1) jointly adding in Low Temperature Thermal reflux, extract, tank by Radix Isatidis and water by the weight ratio of 1:5~15, temperature is 70 degrees Celsius, and vacuum is 0.2 MPa;
(2) add Radix Isatidis and water gross weight 0.1~0.5% sodium chloride, then temperature in extraction pot is risen to 45~75 degrees Celsius and extracts, extraction time is 2~8 hours;
(3) collect extracting solution, under 0.2~0.5 MPa of condition, carry out concentrating under reduced pressure, until relative density is 1.1~1.35 stoppings;
(4) by step product (3) by detergent washing, then collected after centrifugation supernatant under 500~1500 turns of conditions per minute, then supernatant is prepared after 120 degrees Celsius of heated-air circulation oven inner dryings Banlangen Polysaccharide.
The preparation method of above-mentioned Indigowoad root selenium polysaccharide comprises the following steps:
(1) Banlangen Polysaccharide and selenizing agent are added in reactor jointly;
(2) reacting by heating still so that it is interior temperature rises to 40~65 degrees Celsius, adds catalyst;
Step (2) described catalyst is dust technology or barium chloride, and the weight ratio of catalyst and selenizing agent is 0.2~0.45:1, and the catalytic reaction time is 2~12 hours.
(3) centrifugation step product (2) under 500~1500 turns of conditions per minute, then adsorb with the macroporous resin in 100~500 nanometers of aperture;
(4) being washed by step macroporous resin (3) absolute ether, the product of eluting is centrifugal under 500~1500 turns of conditions per minute, and gleanings prepares finished product after drying through heated-air circulation oven;
Embodiment 1
1. prepare Banlangen Polysaccharide
(1) 100 kilograms of Radix Isatidis and 500 kg of water (weight ratio 1:5) jointly being added in Low Temperature Thermal reflux, extract, tank, temperature is 70 degrees Celsius, and vacuum is 0.2 MPa;
(2) adding 0.6 kilogram of sodium chloride (Radix Isatidis and water gross weight 0.1%), then temperature in extraction pot is risen to 45 degrees Celsius and extract, extraction time is 8 hours;
(3) collect extracting solution, under 0.2 MPa of condition, carry out concentrating under reduced pressure, until relative density is 1.1 stoppings;
(4) by the step product (3) 95% washing with alcohol by 3 times, then collected after centrifugation supernatant under 500 turns of conditions per minute, then supernatant is prepared after 120 degrees Celsius of heated-air circulation oven inner dryings Banlangen Polysaccharide.
2. preparation Indigowoad root selenium polysaccharide
(1) 20 kilograms of Banlangen Polysaccharides and 4 kilograms of triphenyls selenizing phosphine (1:0.2) are added in reactor jointly;
(2) reacting by heating still so that it is interior temperature rises to 40 degrees Celsius, adds and the catalyst lean nitric acid that selenizing agent weight ratio is 1:0.2, catalytic reaction 2 hours;
(3) centrifugation step product (2) under 500 turns of conditions per minute, then adsorb with the macroporous resin of 100 nanometers;
(4) being washed by step macroporous resin (3) absolute ether, the product of eluting is centrifugal under 500 turns of conditions per minute, and gleanings prepares finished product after drying through heated-air circulation oven.
Embodiment 2
1. prepare Banlangen Polysaccharide
(1) 50 kilograms of Radix Isatidis and 750 kg of water (weight ratio 1:15) jointly being added in Low Temperature Thermal reflux, extract, tank, temperature is 70 degrees Celsius, and vacuum is 0.2 MPa;
(2) adding 4 kilograms of sodium chloride (Radix Isatidis and water gross weight 0.5%), then temperature in extraction pot is risen to 75 degrees Celsius and extract, extraction time is 2 hours;
(3) collect extracting solution, under 0.5 MPa of condition, carry out concentrating under reduced pressure, until relative density is 1.35 stoppings;
(4) by the absolute ether washing by 5 times of the step product (3), then collected after centrifugation supernatant under 1500 turns of conditions per minute, then supernatant is prepared after 120 degrees Celsius of heated-air circulation oven inner dryings Banlangen Polysaccharide.
2. preparation Indigowoad root selenium polysaccharide
(1) 10 kilograms of Banlangen Polysaccharides and 8.5 kilograms of pyridine-dichloro oxygen selenium (1:0.85) are added in reactor jointly;
(2) reacting by heating still so that it is interior temperature rises to 65 degrees Celsius, adds and the catalyst barium chloride that selenizing agent weight ratio is 1:0.45, catalytic reaction 12 hours;
(3) centrifugation step product (2) under 1500 turns of conditions per minute, then adsorb with the macroporous resin of 500 nanometers;
(4) being washed by step macroporous resin (3) absolute ether, the product of eluting is centrifugal under 1500 turns of conditions per minute, and gleanings prepares finished product after drying through heated-air circulation oven.
Embodiment 3
1. prepare Banlangen Polysaccharide
(1) 80 kilograms of Radix Isatidis and 800 kg of water (weight ratio 1:10) jointly being added in Low Temperature Thermal reflux, extract, tank, temperature is 70 degrees Celsius, and vacuum is 0.2 MPa;
(2) adding 2.64 kilograms of sodium chloride (Radix Isatidis and water gross weight 0.3%), then temperature in extraction pot is risen to 60 degrees Celsius and extract, extraction time is 5 hours;
(3) collect extracting solution, under 0.3 MPa of condition, carry out concentrating under reduced pressure, until relative density is 1.2 stoppings;
(4) by the absolute ether washing by 4 times of the step product (3), then collected after centrifugation supernatant under 1200 turns of conditions per minute, then supernatant is prepared after 120 degrees Celsius of heated-air circulation oven inner dryings Banlangen Polysaccharide.
2. preparation Indigowoad root selenium polysaccharide
(1) 30 kilograms of Banlangen Polysaccharides and 15 kilograms of pyridine-dichloro oxygen selenium (1:0.5) are added in reactor jointly;
(2) reacting by heating still so that it is interior temperature rises to 50 degrees Celsius, adds and the catalyst barium chloride that selenizing agent weight ratio is 1:0.3, catalytic reaction 7 hours;
(3) centrifugation step product (2) under 1200 turns of conditions per minute, then adsorb with the macroporous resin of 300 nanometers;
(4) step macroporous resin (3) absolute ether washs, and the product of eluting is centrifugal under 1200 turns of conditions per minute, and gleanings prepares finished product after drying through heated-air circulation oven.
When prepared by Banlangen Polysaccharide, can increasing the yield of Banlangen Polysaccharide after adding sodium chloride significantly, result is in Table 1:
Table 1: the relation of Banlangen Polysaccharide yield and sodium chloride addition
As seen from the table, Banlangen Polysaccharide preparation process adds the sodium chloride of 0.1~0.5%, it is possible to improve the yield of Banlangen Polysaccharide, wherein add sodium chloride addition and can improve Banlangen Polysaccharide yield 17% when 0.4~0.5% scope.
Indigowoad root selenium polysaccharide ratio in feeding water presses example 1 for 100g/300L, and example 2 be 100g/300L, and example 3 is 100g/300L, respectively test group 1, test group 2, test group 3, matched group is hello Indigowoad root selenium polysaccharide.
Feed 30 days, record the original body mass of every pig, whole opisthosoma weight, with average weight gain, average consumption weight, average feedstuff-meat ratio, mortality rate for Testing index. Table 2 be Indigowoad root selenium polysaccharide to pig weight increment test result, table 3 is that Indigowoad root selenium polysaccharide is to pig resistance against diseases result of the test.
Table 2: Indigowoad root selenium polysaccharide is to pig weight increment test result
Table 3: Indigowoad root selenium polysaccharide is to pig resistance against diseases result of the test
Indigowoad root selenium polysaccharide ratio in feeding water presses example 1 for 100g/300L, and example 2 be 100g/300L, and example 3 is 100g/300L, respectively test group 1, test group 2, test group 3, matched group is hello Indigowoad root selenium polysaccharide.
Feeding 30 days, record turns the Gain weight of group's before and after test object. Table 4 is that Indigowoad root selenium polysaccharide is to pig anti-stress result of the test
Table 4: Indigowoad root selenium polysaccharide is to pig anti-stress result of the test
Indigowoad root selenium polysaccharide ratio in feeding water presses example 1 for 100g/300L, example 2 is 100g/300L, example 3 is 100g/300L, respectively test group 1, test group 2, test group 3, matched group broiler carries out related vaccines immunity and medication by normal aquaculture model, within 42 days, deliver for sale, record Gain weight and the mortality rate of chicken group. Table 5 is that Indigowoad root selenium polysaccharide is to broiler growth result of the test.
Table 5: Indigowoad root selenium polysaccharide is to broiler growth result of the test
Make ambient temperature reach 32 DEG C by infrared heating, and be incubated by thermostat, as high temperature matched group and test group experimental condition. Indigowoad root selenium polysaccharide ratio in feeding water presses example 1 for 100g/300L, and example 2 is 100g/300L, and example 3 is 100g/300L, respectively test group 1, test group 2, test group 3. Feed 30 days, the Gain weight of record chicken group.
Table 6 is the Indigowoad root selenium polysaccharide anti-heat stress result of the test to broiler.
Table 6: the Indigowoad root selenium polysaccharide anti-heat stress result of the test to broiler
Drawing from above experimental result, Indigowoad root selenium polysaccharide can significantly improve the autoimmunity of pig, broiler, increases resistance against diseases.

Claims (4)

1. the preparation method of an Indigowoad root selenium polysaccharide, it is characterized in that: comprise the following steps: its raw material includes Banlangen Polysaccharide and selenizing agent, the weight ratio of the two is 1:0.2~0.85, and described selenizing agent is triphenyl selenizing phosphine, pyridine-dichloro oxygen selenium or sodium selenite;
(1) Banlangen Polysaccharide and selenizing agent are added in reactor jointly;
(2) reacting by heating still so that it is interior temperature rises to 40~65 degrees Celsius, the weight ratio adding catalyst lean nitric acid or barium chloride, catalyst and selenizing agent is 0.2~0.45:1, and the catalytic reaction time is 2~12 hours;
(3) centrifugation step product (2) under 500~1500 turns of conditions per minute, then adsorb with the macroporous resin in 100~500 nanometers of aperture;
(4) being washed by step macroporous resin (3) absolute ether, the product of eluting is centrifugal under 500~1500 turns of conditions per minute, and gleanings prepares finished product through dried;
The preparation method of described Banlangen Polysaccharide comprises the following steps:
1. jointly adding in Low Temperature Thermal reflux, extract, tank by Radix Isatidis and water, temperature is 70 degrees Celsius, and vacuum is 0.2 MPa;
2. add sodium chloride, then temperature in extraction pot is risen to 45~75 degrees Celsius and extract;
3. collect extracting solution, under 0.2~0.5 MPa of condition, carry out concentrating under reduced pressure, until relative density is 1.1~1.35 stoppings;
4. by step product 3. by detergent washing, then collected after centrifugation supernatant under 500~1500 turns of conditions per minute, then supernatant is prepared after 120 degrees Celsius of heated-air circulation oven inner dryings Banlangen Polysaccharide.
2. the preparation method of a kind of Indigowoad root selenium polysaccharide according to claim 1, it is characterised in that: the weight ratio of step 1. described Radix Isatidis and water is 1:5~15.
3. the preparation method of a kind of Indigowoad root selenium polysaccharide according to claim 1, it is characterised in that: addition is Radix Isatidis and water gross weight the 0.1~0.5% of step 2. described sodium chloride, extraction time is 2~8 hours.
4. the preparation method of a kind of Indigowoad root selenium polysaccharide according to claim 1, it is characterised in that: step 4. described detergent is 95% ethanol or absolute ether, and the weight ratio between step product and detergent (3) is 1:3~5.
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Publication number Priority date Publication date Assignee Title
CN101445563A (en) * 2008-10-10 2009-06-03 汤洁 Method for manufacturing selenium-rich fucoidin
CN101654486A (en) * 2009-09-14 2010-02-24 杭州万得富生物技术有限公司 Preparation method of astragalus polysaccharide selenide
CN102532339A (en) * 2012-02-14 2012-07-04 兰州大学 Method for selenizing pilose asiabell root polysaccharides and application of product
CN102653566A (en) * 2012-04-06 2012-09-05 浙江博信药业有限公司 Method for preparing astragalus polysaccharide selenide by using organic method
CN103288973A (en) * 2012-03-02 2013-09-11 中国人民解放军军事医学科学院毒物药物研究所 Isatis root polysaccharides, and preparation method and use thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101445563A (en) * 2008-10-10 2009-06-03 汤洁 Method for manufacturing selenium-rich fucoidin
CN101654486A (en) * 2009-09-14 2010-02-24 杭州万得富生物技术有限公司 Preparation method of astragalus polysaccharide selenide
CN102532339A (en) * 2012-02-14 2012-07-04 兰州大学 Method for selenizing pilose asiabell root polysaccharides and application of product
CN103288973A (en) * 2012-03-02 2013-09-11 中国人民解放军军事医学科学院毒物药物研究所 Isatis root polysaccharides, and preparation method and use thereof
CN102653566A (en) * 2012-04-06 2012-09-05 浙江博信药业有限公司 Method for preparing astragalus polysaccharide selenide by using organic method

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