CN104177514A - Preparation method for improving viscosity of semen plantaginis polysaccharides - Google Patents
Preparation method for improving viscosity of semen plantaginis polysaccharides Download PDFInfo
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- CN104177514A CN104177514A CN201410390932.1A CN201410390932A CN104177514A CN 104177514 A CN104177514 A CN 104177514A CN 201410390932 A CN201410390932 A CN 201410390932A CN 104177514 A CN104177514 A CN 104177514A
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- semen plantaginis
- plantago asiatica
- laccase
- polysaccharides
- asiatica linne
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Abstract
The invention discloses a preparation method for improving viscosity of semen plantaginis polysaccharides. The method comprises the following steps: adding 80% ethanol according to the mass-volume ratio of feed liquid being 1 to 10, and carrying out preprocessing; extracting the preprocessed semen plantaginis in a boiling water bath for 2-3 hours, wherein the mass-volume ratio of the semen plantaginis to water is (1: 10) to (1:30); repeating twice, merging filtrates, concentrating and then adding ethanol to stand for 12 hours at 4 DEG C; controlling the mass concentration of ethanol in the system to be 80%; centrifuging, collecting sediments, and washing twice by using acetone, absolute ether and absolute ethyl alcohol; freezing and drying to obtain semen plantaginis polysaccharides; adding water to re-dissolve the semen plantaginis polysaccharides; adding laccase according to the ratio that 0.1-0.5U of laccase is added to each mg of semen plantaginis polysaccharides; reacting at 25-45 DEG C for 1-8 hours; and freezing and drying to obtain high-viscosity semen plantaginis polysaccharides. The semen plantaginis polysaccharides disclosed by the invention can be directly mixed with the laccase to act, the polysaccharide viscosity is improved, the semen plantaginis polysaccharides are also suitable for other sources of araboxylan polysaccharides, and the prepared high-viscosity semen plantaginis polysaccharides show the shear thinning phenomenon, and have good gel-forming properties.
Description
Technical field
The invention belongs to the preparation of natural product polysaccharide and development technique field.
Background technology
Food fibre refers in human small intestine and can not digestedly absorb, and a class carbohydrate that can partly or entirely be utilized by microorganism in enteron aisle in large intestine can be divided into water-soluble dietary fibre and water insoluble dietary fiber by its solvability.Water-soluble dietary fibre dissolves in warm water or hot water, after absorption, can reduce body inner cholesterol and glucose level, thereby reduces heart disease incidence, improve diabetic symptom.Semen Plantaginis is one of China's medication, first appeared in < < Book of Songs > >, the medicinal beginning is loaded in < < Shennong Bencaojing > >, and be listed in top grade, for before Plantaginaceae plant car (
plantgao asiatical.) or Plantago depressa Willd (
plantago depressawilld.) dry mature seed, has relieving stranguria by diuresis, removing heat to brighten vision, dispels and cough effects such as stopping phlegm, and Xian Bei State Food and Drug Administration classifies the article that can be used for protective foods as.Plantago asiatica linne polyoses is one of outer cell walls main component of Semen Plantaginis kind skin, correlative study in recent years confirmed plantago asiatica linne polyoses have relax bowel, hypoglycemic, regulate the biological activitys such as blood fat, containing the product of psyllium, be also widely used in improving intestinal function and promote that defecation is normal.
Generally believe that at present plantago asiatica linne polyoses intestinal function is relevant with its high viscosity or gel-forming property, but plantago asiatica linne polyoses gellifying property is more weak, such as reports such as British scholar Haque, alkali is carried ispaghul polysaccharide and is shown weak gellifying property, and before this laboratory, the semen plantaginis major water extraction polysaccharide gel-forming property of preparation is not high yet.Therefore improve plantago asiatica linne polyoses viscosity to improve its gel-forming property, significant for the application of plantago asiatica linne polyoses.In addition, high viscosity plantago asiatica linne polyoses can also add in food as thickening material, weighting agent, formulation adjuvant etc., makes various heath food.Chinese patent CN102138981A discloses " a kind of Preparation method and use of plantago asiatica linne polyoses extract ", contriver to raw material degreasing after, through water extraction, alcohol precipitation, obtain Crude polysaccharides again, Crude polysaccharides is sloughed albumen, pigment through dialysis, ion exchange chromatography, remove small molecules chemical composition, prepare the plantago asiatica linne polyoses extract of higher degree.But the preparation method of relevant raising plantago asiatica linne polyoses stickiness has no report.
Summary of the invention
The object of the invention is to provide a kind of preparation method who improves plantago asiatica linne polyoses stickiness, and gained high viscosity polysaccharide apparent viscosity is about 10 ~ 50 times before modification.
The present invention is achieved in that and it is characterized in that method steps is.
(1) Semen Plantaginis pre-treatment: take the Semen Plantaginis of certain mass,, soak 24 hours than adding 80% ethanol for the ratio of 1:10 in feed liquid quality volume (kg/L), filter, collect Semen Plantaginis, dry.
(2) plantago asiatica linne polyoses preparation: take the Semen Plantaginis that a certain amount of step (1) is processed, extract 2 ~ 3 hours under boiling water bath, the quality volume (kg/L) of Semen Plantaginis and water, than for 1:10 ~ 1:30, is collected filtrate after extracting liquid filtering, and filter residue repeats to extract 1 time.Merge filtrate twice, concentrating under reduced pressure, adds ethanol standing 12 hours in 4 ℃ in concentrated solution, ethanol mass concentration in system is controlled at 80%, centrifugal, collecting precipitation, precipitation is used acetone, anhydrous diethyl ether, each washed twice of dehydrated alcohol successively, and then sample obtains plantago asiatica linne polyoses through lyophilize.
(3) plantago asiatica linne polyoses enzymatic treatment: take the resulting plantago asiatica linne polyoses of a certain amount of step (2), adding water redissolves, then according to every milligram of plantago asiatica linne polyoses correspondence, add the ratio of 0.1 ~ 0.5 U laccase to add laccase, at 25 ~ 45 ℃, react 1 ~ 8 hour, reaction finishes postlyophilization, obtains high viscosity plantago asiatica linne polyoses.
Plantago asiatica linne polyoses enzymatic treatment of the present invention directly adds laccase in plantago asiatica linne polyoses solution, after reaction certain hour, can obtain high viscosity plantago asiatica linne polyoses.
Plantago asiatica linne polyoses enzymatic treatment of the present invention, laccase activity unit >=0.5 U/mg, laccase addition corresponding to every milligram of plantago asiatica linne polyoses be 0.4 ~ 0.5 U preferably, laccase and preferably 2 ~ 4 hours action time of polysaccharide, preferably 25 ℃ ~ 40 ℃ of laccase and polysaccharide operative temperatures.
Plantago asiatica linne polyoses enzymatic treatment of the present invention, the plantago asiatica linne polyoses viscosity after laccase effect has improved approximately 10 ~ 50 times.
Plantago asiatica linne polyoses of the present invention, is characterized in that described plantago asiatica linne polyoses is a kind of water-soluble, araboxylan class polysaccharide, so other source araboxylan class polysaccharide are also applicable to present method.
Advantage of the present invention is: 1, plantago asiatica linne polyoses can be directly and after laccase mixing effect for some time, just can greatly improve polysaccharide viscosity; 2, present method plantago asiatica linne polyoses used, is a kind of water-soluble, araboxylan class polysaccharide, is therefore also applicable to other source araboxylan class polysaccharide; 3, the high viscosity plantago asiatica linne polyoses preparing, presents shear shinning phenomenon, has good gel-forming property, can be used as thickening material and is applied in food, makeup, medicine industry.
Embodiment
In conjunction with following specific embodiment, the present invention is described in further detail.Implement process of the present invention, condition, reagent, experimental technique etc., except the content of mentioning specially below, be the universal knowledege of this area, the present invention is not particularly limited content.
Viscosity measurement method of the present invention is: use ARES-G2 rotational rheometer (U.S. TA Instrument company), fixture is 40 mm parallel plates, and probe temperature is 25 ℃, and shearing rate scan scope is 0.1 ~ 500 s
-1.Obtain the apparent viscosity of sample along with shear rate change curve, getting shearing rate on curve is 0.125 s
-1apparent viscosity as investigating index.
Embodiment 1.
Take and be dried semen plantaginis major as raw material, take 100 g Semen Plantaginiss, in feed liquid quality volume (kg/L), than adding 80% alcohol immersion 24 hours for the ratio of 1:10, two-layer filtered through gauze, dries.
Take a certain amount of Semen Plantaginis crossing through alcohol immersion, extract 3 hours under boiling water bath, the mass volume ratio of Semen Plantaginis and water is 1:10, collects filtrate after extracting liquid filtering, and filter residue repeats to extract 1 time.Merge filtrate twice, concentrating under reduced pressure, adds ethanol standing 12 hours in 4 ℃ in concentrated solution, ethanol mass concentration in system is controlled at 80%, centrifugal, collecting precipitation, precipitation is used acetone, anhydrous diethyl ether, each washed twice of dehydrated alcohol successively, and then sample obtains plantago asiatica linne polyoses through lyophilize.
Gained plantago asiatica linne polyoses sample preparation is become to 0.5% plantago asiatica linne polyoses solution, then according to every milligram of plantago asiatica linne polyoses correspondence, add the ratio of 0.3 U laccase to add laccase, in 25 ℃ of thermostat water baths standing 2 hours.According to above-mentioned condition, do same treatment, but do not add laccase, obtain control sample simultaneously.Adopt Ares rheometer, the polysaccharide of measuring after laccase effect is 0.125 s in 25 ℃ of temperature, shearing rate
-1time, its apparent viscosity is 1.40 Pas, and contrast plantago asiatica linne polyoses sample apparent viscosity is 0.16 Pa*s, and viscosity has increased approximately 8 times.
Embodiment 2.
Take and be dried semen plantaginis major as raw material, take 100 g Semen Plantaginiss, in feed liquid quality volume (kg/L), than adding 80% ethanol 24 hours for the ratio of 1:10, two-layer filtered through gauze, dries.
Take a certain amount of Semen Plantaginis crossing through alcohol immersion, extract 3 hours under boiling water bath, the mass volume ratio of Semen Plantaginis and water is 1:10, collects filtrate after extracting liquid filtering, and filter residue repeats to extract 1 time.Merge filtrate twice, concentrating under reduced pressure, adds ethanol standing 12 hours in 4 ℃ in concentrated solution, ethanol mass concentration in system is controlled at 80%, centrifugal, collecting precipitation, precipitation is used acetone, anhydrous diethyl ether, each washed twice of dehydrated alcohol successively, and then sample obtains plantago asiatica linne polyoses through lyophilize.
Gained plantago asiatica linne polyoses sample preparation is become to 1% plantago asiatica linne polyoses solution, then according to every milligram of plantago asiatica linne polyoses correspondence, add the ratio of 0.4 U laccase to add laccase, in 25 ℃ of thermostat water baths standing 2 hours.According to above-mentioned condition, do same treatment, but do not add laccase, obtain control sample simultaneously.Adopt Ares rheometer, the polysaccharide of measuring after laccase effect is 0.125 s in 25 ℃ of temperature, shearing rate
-1time, its apparent viscosity is 40.64 Pas, and contrast plantago asiatica linne polyoses sample apparent viscosity is 1.28 Pa*s, and viscosity has increased approximately 32 times.
Embodiment 3.
Take and be dried semen plantaginis major as raw material, take 100 g Semen Plantaginiss, in feed liquid quality volume (kg/L), than adding 80% alcohol immersion 24 hours for the ratio of 1:10, two-layer filtered through gauze, dries.
Take a certain amount of Semen Plantaginis crossing through alcohol immersion, extract 3 hours under boiling water bath, the mass volume ratio of Semen Plantaginis and water is 1:10, collects filtrate after extracting liquid filtering, and filter residue repeats to extract 1 time.Merge filtrate twice, concentrating under reduced pressure, adds ethanol standing 12 hours in 4 ℃ in concentrated solution, ethanol mass concentration in system is controlled at 80%, centrifugal, collecting precipitation, precipitation is used acetone, anhydrous diethyl ether, each washed twice of dehydrated alcohol successively, and then sample obtains plantago asiatica linne polyoses through lyophilize.
Gained plantago asiatica linne polyoses sample preparation is become to 1% plantago asiatica linne polyoses solution, then according to every milligram of plantago asiatica linne polyoses correspondence, add the ratio of 0.4 U laccase to add laccase, in 25 ℃ of thermostat water baths standing 6 hours.According to above-mentioned condition, do same treatment, but do not add laccase, obtain control sample simultaneously.Adopt Ares rheometer, the polysaccharide of measuring after laccase effect is 0.125 s in 25 ℃ of temperature, shearing rate
-1time, its apparent viscosity is 15.55 Pas, and contrast plantago asiatica linne polyoses sample apparent viscosity is 1.14 Pa*s, and viscosity has increased approximately 14 times.
Embodiment 4.
Take and be dried semen plantaginis major as raw material, take 100 g Semen Plantaginiss, in feed liquid quality volume (kg/L), than adding 80% alcohol immersion 24 hours for the ratio of 1:10, two-layer filtered through gauze, dries.
Take a certain amount of Semen Plantaginis crossing through alcohol immersion, extract 3 hours under boiling water bath, the mass volume ratio of Semen Plantaginis and water is 1:10, collects filtrate after extracting liquid filtering, and filter residue repeats to extract 1 time.Merge filtrate twice, concentrating under reduced pressure, adds ethanol standing 12 hours in 4 ℃ in concentrated solution, ethanol mass concentration in system is controlled at 80%, centrifugal, collecting precipitation, precipitation is used acetone, anhydrous diethyl ether, each washed twice of dehydrated alcohol successively, and then sample obtains plantago asiatica linne polyoses through lyophilize.
Gained plantago asiatica linne polyoses sample preparation is become to 1% plantago asiatica linne polyoses solution, then according to every milligram of plantago asiatica linne polyoses correspondence, add the ratio of 0.4 U laccase to add laccase, in 40 ℃ of thermostat water baths standing 2 hours.According to above-mentioned condition, do same treatment, but do not add laccase, obtain control sample simultaneously.Adopt Ares rheometer, the polysaccharide of measuring after laccase effect is 0.125 s in 25 ℃ of temperature, shearing rate
-1time, its apparent viscosity is 18.02 Pas, and contrast plantago asiatica linne polyoses sample apparent viscosity is 0.62 Pa*s, and viscosity has increased approximately 29 times.
Claims (3)
1. improve a preparation method for plantago asiatica linne polyoses stickiness, it is characterized in that as follows:
(1) Semen Plantaginis pre-treatment: take the Semen Plantaginis of certain mass,, soak 24 hours than adding 80% ethanol for the ratio of 1:10 in feed liquid quality volume (kg/L), filter, collect Semen Plantaginis, dry;
(2) plantago asiatica linne polyoses preparation: take the Semen Plantaginis that a certain amount of step (1) is processed, extract 2 ~ 3 hours under boiling water bath, the mass volume ratio of Semen Plantaginis and water (kg/L) is 1:10 ~ 1:30, collects filtrate after extracting liquid filtering, and filter residue repeats to extract 1 time; Merge filtrate twice, concentrating under reduced pressure, adds ethanol standing 12 hours in 4 ℃ in concentrated solution, ethanol mass concentration in system is controlled at 80%, centrifugal, collecting precipitation, precipitation is used acetone, anhydrous diethyl ether, each washed twice of dehydrated alcohol successively, through lyophilize, obtains plantago asiatica linne polyoses;
(3) plantago asiatica linne polyoses enzymatic treatment: take the resulting plantago asiatica linne polyoses of a certain amount of step (2), adding water redissolves, then according to every milligram of plantago asiatica linne polyoses, add the ratio of 0.1 ~ 0.5 U laccase to add laccase, at 25 ~ 45 ℃, react 1 ~ 8 hour, reaction finishes postlyophilization, obtains high viscosity plantago asiatica linne polyoses.
2. the preparation method of raising plantago asiatica linne polyoses stickiness according to claim 1, is characterized in that directly in plantago asiatica linne polyoses solution, adding laccase.
3. the preparation method of raising plantago asiatica linne polyoses stickiness according to claim 1, it is characterized in that laccase activity unit >=0.5 U/mg, every milligram of laccase addition corresponding to plantago asiatica linne polyoses is 0.4 ~ 0.5 U, laccase and polysaccharide action time are 2 ~ 4 hours, and laccase and polysaccharide operative temperature are 25 ℃ ~ 40 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926952A (en) * | 2015-06-10 | 2015-09-23 | 南昌大学 | Method for preparing arabinoxylan from semen plantaginis |
| CN114592019A (en) * | 2022-04-06 | 2022-06-07 | 厦门爱逸零食研究所有限公司 | Method for preparing oligosaccharide by combining plantain seed polysaccharide and application thereof |
| CN115926199A (en) * | 2022-12-07 | 2023-04-07 | 盐城工学院 | Preparation method of self-repairing conductive ionic hydrogel |
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| CN101756172A (en) * | 2009-12-21 | 2010-06-30 | 南昌大学 | Method for preparing soluble plantain seed dietary fiber and application thereof |
| CN102138981A (en) * | 2011-04-01 | 2011-08-03 | 匡海学 | Preparation method of plantago seed polysaccharide extractive and applications thereof |
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2014
- 2014-08-11 CN CN201410390932.1A patent/CN104177514A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101756172A (en) * | 2009-12-21 | 2010-06-30 | 南昌大学 | Method for preparing soluble plantain seed dietary fiber and application thereof |
| CN102138981A (en) * | 2011-04-01 | 2011-08-03 | 匡海学 | Preparation method of plantago seed polysaccharide extractive and applications thereof |
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| 周超 等: "车前子多糖的测定方法研究", 《分析试验室》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104926952A (en) * | 2015-06-10 | 2015-09-23 | 南昌大学 | Method for preparing arabinoxylan from semen plantaginis |
| CN114592019A (en) * | 2022-04-06 | 2022-06-07 | 厦门爱逸零食研究所有限公司 | Method for preparing oligosaccharide by combining plantain seed polysaccharide and application thereof |
| CN114592019B (en) * | 2022-04-06 | 2023-08-15 | 厦门爱逸零食研究所有限公司 | Method for preparing oligosaccharide by combining Plantago ovata polysaccharide and application thereof |
| CN115926199A (en) * | 2022-12-07 | 2023-04-07 | 盐城工学院 | Preparation method of self-repairing conductive ionic hydrogel |
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Application publication date: 20141203 |