CN107793491A - A kind of preparation method of squid ink polysaccharide oligosaccharides - Google Patents
A kind of preparation method of squid ink polysaccharide oligosaccharides Download PDFInfo
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Abstract
A kind of preparation method of squid ink polysaccharide oligosaccharides, described preparation method include：（1）Squid prepared Chinese ink adds isometric 10 ~ 12h of distilled water immersion, centrifugation, takes supernatant；After sediment fraction adds 2 times of volume distillation water washings, repeated centrifugation, merge the supernatant centrifuged twice；（2）Papain is added in squid ink supernatant and neutral proteinase carries out complex enzyme hydrolysis, and batch (-type) is with ultrasonication auxiliary enzymes；（3）After enzyme digestion reaction terminates, 95 ~ 100 DEG C of enzyme deactivation 10min, centrifuge to remove impurity, the absolute ethyl alcohol that 4 ~ 4.5 times of volumes are added in supernatant precipitates to squid ink polysaccharide, and sediment fraction is squid ink polysaccharide；（4）Squid ink polysaccharide is soluble in water, it is placed in microwave device and carries out microwave treatment；5）Solution after microwave treatment carries out ultrasonication；Resulting solution is dialysed through bag filter removes micromolecular compound, after vacuum freeze drying, obtains squid ink polysaccharide oligosaccharides.
Description
Technical field
The present invention relates to a kind of preparation method of the squid ink polysaccharide oligosaccharides with hypoglycemic effect, belong to squid leftover bits and pieces
The processing technique field of squid ink.
Background technology
Squid is one of marine living resources that amount of fishing is most in the world, and China is up to tens of to the year amount of fishing of squid
Ten thousand tons.Squid ink is the leftover bits and pieces of squid secondary industry, accounts for the 1.3% of squid body weight.Squid ink is swung in medicinal aspect history
Long,《Bencao Shiyi》Frightened squid ink, puckery are recorded, enters the heart channel of Hang-Shaoyin, activate blood circulation and disperse blood clots, cooling blood and hemostasis.Squid ink is used as one in Japan
Kind important food and health products raw material is widely used, and China at present the utilization rate to squid ink and it is high-valued it is horizontal compared with
Low, the bioactive substance enriched in squid ink is not yet preferably utilized, and both pollutes environment, and waste of resource.Modern times doctor
Research is learned it was demonstrated that squid ink has antitumor, raising immunity, anti-inflammatory, radioresistance and promotees the effect such as blood coagulation.Therefore, will
Squid ink carries out intensive processing, turns waste into wealth, and promotes the higher value application of squid ink resource, has higher economic value and society
Can benefit.
Squid ink polysaccharide is one of functional compound main in squid ink, and it is to be combined into peptide polysaccharide with protein peptides
Form exist, carbohydrate fraction mainly contains the gluconic acid of decile protonatomic mass, N- acetylgalactosamines, fucosan etc.；Peptide
The composition amino acid of chain part includes：Aspartic acid, threonine, serine, glutamic acid, alanine.It is proved squid ink at present
Polysaccharide has the bioactivity such as antitumor, raising immunity, anti-gastric-ulcer, protection intestinal mucosa.At present to squid ink polysaccharide
Extraction is mainly to utilize lipase using alcohol deposition method, such as patent " a kind of squid prepared Chinese ink polysaccharide and preparation method thereof " is digested
Complex enzyme hydrolysis is carried out to squid prepared Chinese ink with papain, recycles ethanol or acetone that the side of polysaccharide is precipitated or obtained to polysaccharide
Method.The advantages of this method is that separation and extraction are easier, but enzymolysis and extraction rate is not high, and albumen removal is not thorough enough, in addition also
The pure acetone of chemistry is introduced, there is the risk for introducing organic solvent.Such as paper again《The research of squid ink polysaccharide and melanin》,
It is to remove unnecessary albumen using papain enzymolysis twice, ethanol precipitation polysaccharide, trichloroacetic acid, obtains polysaccharide.This method
The advantages of be after trichloroacetic acid deproteination, the protein content in polysaccharide product significantly reduces, but enzymolysis efficiency is not still high.
In addition, the molecular weight of squid ink polysaccharide is larger, average molecular weight is up to 50~60KDa, is unfavorable for absorption of human body, is ensureing polysaccharide chain
In the case of constant, polysaccharide is degraded to oligosaccharides, human body can be greatly facilitated oligosaccharides is absorbed.At present, it there is no squid
The research report of fish ink polysaccharide oligosaccharides.
The content of the invention
The invention aims to solve the deficiencies in the prior art, there is provided a kind of method is easy, is easily given birth to
Production control, it is avoided that organic solvent introduces the potential safety hazard brought, the ratio that oligosaccharides is absorbed by the body can be improved, increase squid ink
The specific activity of polysaccharide oligosaccharides, the preparation method of the higher squid ink polysaccharide oligosaccharides with hypoglycemic effect of recovery rate.
The purpose of the present invention is completed by following technical solution, a kind of preparation method of squid ink polysaccharide oligosaccharides,
, using squid prepared Chinese ink as raw material, described preparation method comprises the following steps for it：
(1) squid prepared Chinese ink adds isometric 10~12h of distilled water immersion, 4,500r/min 10~15min of centrifugation, takes
Clear liquid；After sediment fraction adds 2 times of volume distillation water washings, repeated centrifugation, merge the supernatant centrifuged twice；
(2) addition papain and neutral proteinase progress complex enzyme hydrolysis in the squid ink supernatant of acquirement, and
Formula of having a rest is with ultrasonication auxiliary enzymes；
(3) after enzyme digestion reaction terminates, 95~100 DEG C of enzyme deactivation 10min, 7,500r/min 15~20min of centrifugation are with except impurity elimination
Matter, the absolute ethyl alcohol that 4~4.5 times of volumes are added in supernatant precipitate to squid ink polysaccharide, stand 30min, and 7,500r/
Min centrifuges 10~15min, takes precipitation, 10~12% solution of trichloroacetic acid for being precipitated and dissolved in 10 times of volumes is unnecessary to remove
Protein, 2h is stood at room temperature, 7,500r/min 10~15min of centrifugation, sediment fraction is squid ink polysaccharide；
(4) it is squid ink polysaccharide is soluble in water, it is placed in microwave device, carries out microwave treatment at a temperature of 60~80 DEG C, 400
~600W handles 10~20min.
(5) solution after microwave treatment carries out ultrasonication, 50~70min of processing time at a temperature of 50~60 DEG C, surpasses
Several field intensities are 200~400W/cm2, supersonic frequency is 20~25kHz；Resulting solution is dialysed through 1,000 molecular weight bag filters
Micromolecular compound is removed, crosses the pvdf membrane of 8,000 molecular weight interception to remove macromolecular compound, vacuum freeze drying
Afterwards, squid ink polysaccharide oligosaccharides is obtained.
As preferred：In described step (3), papain addition is 12,000~16,000U/L squid prepared Chinese ink
Supernatant, neutral proteinase addition are 5,000~9,000U/L squid prepared Chinese ink supernatants, 40~60 DEG C of hydrolysis temperature, pH value 7
~9,3~5h of enzyme digestion reaction time；Enzyme digestion reaction starts, strong with 5~30min of ultrasound-assisted enzymolysis, ultrasonic sound field every 1h
Spend for 60W/cm2, supersonic frequency is 20~25kHz.
The present invention digests squid prepared Chinese ink using squid prepared Chinese ink as raw material, using acid protease enzymatic isolation method, and utilizes ultrasonic wave
Batch (-type) assistance enzymolysis, ethanol precipitation obtain squid ink polysaccharide, trichloroacetic acid deproteination.The squid ink polysaccharide of acquisition is through micro-
Ripple first post-processes with ultrasonic wave, destroys the glycosidic bond of sugar chain, and acquisition molecular weight is smaller, is easily absorbed by the human body, the squid that activity is stronger
Fish ink polysaccharide oligosaccharides, the active relatively low and larger composition of molecular weight is removed using UF membrane, further increases squid ink polysaccharide
The purity and Rate activity of oligosaccharides.This will greatly improve the application value of squid ink, be effectively increased the economy of squid processing fent
Value, promote the development of squid secondary industry.
Compared with prior art, it is of the invention to have the prominent advantages that：
1st, squid ink polysaccharide is separated using ultrasonic assistant complex enzyme zymohydrolysis method, enzymolysis efficiency is high, and method is easy, easily carries out
Production control, and the potential safety hazard that the introducing for avoiding organic solvent is brought.
2nd, glycosidic bond is broken by ultrasonic-microwave combined degradation method, degraded squid ink polysaccharide is oligosaccharides, to product structure
Small, no side reaction is destroyed, reaction is gentle, the molecular weight of easily controllable oligosaccharides.
3rd, understood according to existing scientific achievement：The squid ink polysaccharide oligosaccharides of gained of the invention is compared with natural squid ink polysaccharide
Compared with, because its molecular weight is low, and be more beneficial for absorption of human body, function of reducing blood sugar bioactivity also indicates that, the present invention gained squid ink it is more
The squid ink polysaccharide of sugared oligosaccharide ratio present invention gained has stronger bioactivity, can be applied to corresponding health products, function food
The industry such as product or medical formula food, there is high society, economic implications and application potential.
Specific implementation method
The present invention is described in further detail with reference to embodiments.A kind of preparation method of squid ink polysaccharide oligosaccharides,
, using squid prepared Chinese ink as raw material, described preparation method comprises the following steps for it：
(1) squid prepared Chinese ink adds isometric 10~12h of distilled water immersion, 4,500r/min 10~15min of centrifugation, takes
Clear liquid；After sediment fraction adds 2 times of volume distillation water washings, repeated centrifugation, merge the supernatant centrifuged twice；
(2) addition papain and neutral proteinase progress complex enzyme hydrolysis in the squid ink supernatant of acquirement, and
Formula of having a rest is with ultrasonication auxiliary enzymes；
(3) after enzyme digestion reaction terminates, 95~100 DEG C of enzyme deactivation 10min, 7,500r/min 15~20min of centrifugation are with except impurity elimination
Matter, the absolute ethyl alcohol that 4~4.5 times of volumes are added in supernatant precipitate to squid ink polysaccharide, stand 30min, and 7,500r/
Min centrifuges 10~15min, takes precipitation, 10~12% solution of trichloroacetic acid for being precipitated and dissolved in 10 times of volumes is unnecessary to remove
Protein, 2h is stood at room temperature, 7,500r/min 10~15min of centrifugation, sediment fraction is squid ink polysaccharide；
(4) it is squid ink polysaccharide is soluble in water, it is placed in microwave device, carries out microwave treatment at a temperature of 60~80 DEG C, 400
~600W handles 10~20min.
(5) solution after microwave treatment carries out ultrasonication, 50~70min of processing time at a temperature of 50~60 DEG C, surpasses
Several field intensities are 200~400W/cm2, supersonic frequency is 20~25kHz；Resulting solution is dialysed through 1,000 molecular weight bag filters
Micromolecular compound is removed, crosses the pvdf membrane of 8,000 molecular weight interception to remove macromolecular compound, vacuum freeze drying
Afterwards, squid ink polysaccharide oligosaccharides is obtained.
In described step (3), papain addition is 12,000~16,000U/L squid prepared Chinese ink supernatants, in
Property protease addition be 5,000~9,000U/L squid prepared Chinese ink supernatants, 40~60 DEG C of hydrolysis temperature, pH value 7~9, enzymolysis
3~5h of reaction time；Enzyme digestion reaction starts, and every 1h with 5~30min of ultrasound-assisted enzymolysis, ultrasonic sound field intensity is 60W/
cm2, supersonic frequency is 20~25kHz.
Embodiment 1
(1) squid prepared Chinese ink adds isometric distilled water immersion 10h, 4,500r/min centrifugation 15min, takes supernatant；It is heavy
Form sediment after 2 times of volumes distillation water washings of part addition, repeated centrifugation, merge the supernatant centrifuged twice.
(2) addition papain and neutral proteinase progress complex enzyme hydrolysis in the squid ink supernatant of acquirement, and
Formula of having a rest is with ultrasonication auxiliary enzymes.Wherein, papain addition is 14,000U/L squid prepared Chinese ink supernatants, neutral egg
White enzyme addition is 7,000U/L squid prepared Chinese ink supernatants, 55 DEG C of hydrolysis temperature, pH value 7.5, enzyme digestion reaction time 5h；Enzymolysis is anti-
It should start, every 1h with ultrasound-assisted enzymolysis 10min, ultrasonic sound field intensity is 60W/cm2, supersonic frequency is 20~25kHz.
(3) after enzyme digestion reaction terminates, 95~100 DEG C of enzyme deactivation 10min, 7,500r/min centrifuge 15min to remove impurity, on
The absolute ethyl alcohol that 4 times of volumes are added in clear liquid precipitates to squid ink polysaccharide, stands 30min, 7,500r/min centrifugations
15min, precipitation is taken, be precipitated and dissolved in 12% solution of trichloroacetic acid of 10 times of volumes to remove excess protein matter, it is quiet at room temperature
2h is put, 7,500 r/min centrifugation 15min, sediment fraction is squid ink polysaccharide.
(4) it is squid ink polysaccharide is soluble in water, it is placed in microwave device, carries out microwave treatment at a temperature of 70 DEG C, at 500W
Manage 15min,
(5) solution after microwave treatment carries out ultrasonication, processing time 60min at a temperature of 55 DEG C, and ultrasonic sound field is strong
Spend for 300W/cm2, supersonic frequency is 20~25kHz.Resulting solution is dialysed through 1,000 molecular weight bag filters and removes small molecule
Compound, the pvdf membrane of 8,000 molecular weight interception is crossed to remove macromolecular compound, after vacuum freeze drying, it is more to obtain squid ink
Sugared oligosaccharides.
In embodiment 1 (3), calculated with the squid ink polysaccharide of acquisition than actual more saccharometers in squid ink, squid ink polysaccharide carries
It is 92.4% to take rate.In embodiment 1 (5), with the molecular weight 1 of acquisition, 000~8,000Da squid ink polysaccharide oligosaccharide ratio squid inks
Polysaccharide meter, it is 81.1% that oligosaccharides, which prepares yield,.
Embodiment 2
To verify influence of the addition of papain in the step of embodiment 1 (2) to squid ink polysaccharide extract rate, surround
The addition of different papains, experiment of single factor is designed, remaining is more so as to obtain corresponding squid ink with embodiment 1
Sugared recovery rate, as shown in table 1.
The different papain additions of table 1 are for squid ink polysaccharide extract rate
By table 4 it can be found that papain addition is at 12,000~14,000U/L changes, gained squid ink is more
Sugared recovery rate is in increase trend, and papain addition is in 14, when 000~16,000U/L changes, squid ink polysaccharide extract rate
It is basically unchanged, and gained squid ink polysaccharide extract rate is about 92.4%.
Embodiment 3
To verify influence of the addition of neutral proteinase in the step of embodiment 1 (2) to squid ink polysaccharide extract rate, surround
The addition of different neutral proteinases, experiment of single factor is designed, remaining is more so as to obtain corresponding squid ink with embodiment 1
Sugared recovery rate, as shown in table 2.
The different neutral proteinase additions of table 2 are for squid ink polysaccharide extract rate
By table 2 it can be found that neutral proteinase addition is in 5, when 000~8,000U/L changes, gained squid ink polysaccharide
Recovery rate is in increase trend, and for neutral proteinase addition at 8,000~9,000U/L changes, squid ink polysaccharide extract rate is basic
It is constant, and gained squid ink polysaccharide extract rate is about 93.5%.
Embodiment 4
To verify influence of the hydrolysis temperature to squid ink polysaccharide extract rate in the step of embodiment 1 (2), around different enzymolysis
Temperature, experiment of single factor is designed, remaining is with embodiment 1, so as to squid ink polysaccharide extract rate corresponding to obtaining, as shown in table 3.
3 different hydrolysis temperatures of table are for squid ink polysaccharide extract rate
By table 3 it can be found that hydrolysis temperature is when changing for 40~50 DEG C, gained squid ink polysaccharide extract rate becomes in increase
Gesture, when changing for 40~50 DEG C, squid ink polysaccharide extract rate is basically unchanged hydrolysis temperature, and gained squid ink polysaccharide extract rate is about
For 92.3%.
Embodiment 5
To digest influence of the pH value to squid ink polysaccharide extract rate in the checking step of embodiment 1 (2), around different pH
Value, experiment of single factor is designed, remaining is with embodiment 1, so as to squid ink polysaccharide extract rate corresponding to obtaining, as shown in table 4.
The pH value of table 4 is for squid ink polysaccharide extract rate
By table 4 it can be found that pH value is when 7~7.5 change, gained squid ink polysaccharide extract rate is in increase trend, enzymolysis
When 7.5~8 change, squid ink polysaccharide extract rate is basically unchanged temperature, and gained squid ink polysaccharide extract rate is about 92.4%
For hydrolysis temperature when 8~9 change, squid ink polysaccharide extract rate is on a declining curve.
Embodiment 6
To verify influence of the enzymolysis time to squid ink polysaccharide extract rate in the step of embodiment 1 (2), around different enzymolysis
Time, experiment of single factor is designed, remaining is with embodiment 1, so as to squid ink polysaccharide extract rate corresponding to obtaining, as shown in table 5.
5 different enzymolysis times of table are for squid ink polysaccharide extract rate
By table 5 it can be found that enzymolysis time is when 3~4h changes, gained squid ink polysaccharide extract rate is in increase trend, enzyme
The time is solved when 3~4h changes, squid ink polysaccharide extract rate is basically unchanged, and gained squid ink polysaccharide extract rate is about
92.3%.
Embodiment 7
To verify influence of the ultrasonic wave added enzymolysis time to squid ink polysaccharide extract rate in the step of embodiment 1 (2), around not
With sonication times, design experiment of single factor, remaining is with embodiment 1, so as to squid ink polysaccharide extract rate corresponding to obtaining, such as
Shown in table 6.
6 different hydrolysis temperatures of table are for squid ink polysaccharide extract rate
By table 6 it can be found that ultrasonic wave added enzymolysis time is when 5~10min changes, gained squid ink polysaccharide extract rate is in
Increase trend, when 10~15min changes, squid ink polysaccharide extract rate is basically unchanged ultrasonic wave added enzymolysis time, and gained squid
Fish ink polysaccharide extract rate is about 92.5%, and for ultrasonic wave added enzymolysis time when 15~30min changes, squid ink polysaccharide extract rate is anxious
Speed declines, it may be possible to the structure of enzyme is destroyed because ultrasonic time is long.
Embodiment 8
It is to verify that microwave treatment factor is to the shadow of the squid ink polysaccharide oligosaccharides yield prepared in the step of embodiment 1 (4)
Ring, three factors of temperature, processing time and microwave intensity in step (4), design Three factors-levels orthogonal experiment,
Remaining is with embodiment 1, so as to squid ink polysaccharide oligosaccharides yield amount corresponding to obtaining, as shown in table 7.
Squid ink polysaccharide oligosaccharides yield obtained by the microwave treatment of the different temperatures of table 7, processing time and microwave intensity
By table 7 it can be found that temperature 70 C, processing time 15min, microwave treatment that intensity is 500W and temperature 70 C,
Processing time 25min, intensity are 400W microwave treatment；80 DEG C of temperature, processing time 15min, intensity are at 400W microwave
Reason；80 DEG C of temperature, processing time 25min, intensity are 600W microwave treatment, and gained squid ink polysaccharide oligosaccharides yield is suitable,
Highest in orthogonal experiment, about 81.4%.
Embodiment 9
It is ultrasonication factor in the checking step of embodiment 1 (5) to the squid ink polysaccharide oligosaccharides yield for preparing
Influence, three factors of temperature, processing time and ultrasonic sound field intensity in step (5), design Three factors-levels are just
Experiment is handed over, remaining is with embodiment 1, so as to squid ink polysaccharide oligosaccharides yield corresponding to obtaining, as shown in table 8.
Squid ink polysaccharide oligosaccharides yield obtained by the ultrasonication of the different temperatures of table 8, processing time and ultrasonic sound field intensity
By table 8 it can be found that temperature 60 C, processing time 70min, sound field intensity 400W/cm2Ultrasonic pretreatment
Under, squid ink polysaccharide oligosaccharides yield highest, it is 82.3%.
Embodiment 10
To verify the hypoglycemic activity of squid ink polysaccharide oligosaccharides, C57BL/J mouse are established using high lipid food feeding method
Hyperglycemia model, feed squid ink polysaccharide and squid ink polysaccharide oligosaccharides 80mg/kg body weight respectively daily, it is lasting to carry out
13 weeks, detection mouse fasting blood-glucose, glycosylated hemoglobin and oral glucose tolerance amount situation of change were more so as to obtain squid ink
The hypoglycemic activity of sugared oligosaccharides, as shown in table 9.
Effect of the squid ink polysaccharide oligosaccharides of table 9 to hyperglycaemia mouse fasting blood-glucose and glycosylated hemoglobin
Note：##P ﹤ 0.01, compared with normal group；*P ﹤ 0.05,**P ﹤ 0.01, compared with module.
Claims (2)
1. a kind of preparation method of squid ink polysaccharide oligosaccharides, it is using squid prepared Chinese ink as raw material, it is characterised in that described preparation side
Method comprises the following steps：
（1）Squid prepared Chinese ink adds isometric distilled water immersion 10 ~ 12h, 4,500 r/min 10 ~ 15min of centrifugation, takes supernatant；
After sediment fraction adds 2 times of volume distillation water washings, repeated centrifugation, merge the supernatant centrifuged twice；
（2）Papain is added in the squid ink supernatant of acquirement and neutral proteinase carries out complex enzyme hydrolysis, and batch (-type)
With ultrasonication auxiliary enzymes；
（3）After enzyme digestion reaction terminates, 95 ~ 100 DEG C of enzyme deactivations 10min, 7,500 r/min centrifuge 15 ~ 20min to remove impurity, on
The absolute ethyl alcohol that 4 ~ 4.5 times of volumes are added in clear liquid precipitates to squid ink polysaccharide, stands 30min, 7,500 r/min centrifugations
10 ~ 15min, precipitation is taken, be precipitated and dissolved in 10 ~ 12% solution of trichloroacetic acid of 10 times of volumes to remove excess protein matter, room temperature
Lower standing 2h, 7,500 r/min centrifuge 10 ~ 15min, and sediment fraction is squid ink polysaccharide；
（4）Squid ink polysaccharide is soluble in water, it is placed in microwave device, microwave treatment, 400 ~ 600W is carried out at a temperature of 60 ~ 80 DEG C
Handle 10 ~ 20min；
（5）Solution after microwave treatment carries out ultrasonication, 50 ~ 70min of processing time at a temperature of 50 ~ 60 DEG C, ultrasonic sound field
Intensity is 200 ~ 400W/cm2, supersonic frequency is 20 ~ 25kHz；Resulting solution removes small point through the dialysis of 1,000 molecular weight bag filters
Sub- compound, the pvdf membrane of 8,000 molecular weight interception is crossed to remove macromolecular compound, after vacuum freeze drying, obtains squid
Black polysaccharide oligosaccharides.
2. the preparation method of squid ink polysaccharide oligosaccharides according to claim 1, it is characterised in that described step（3）In,
Papain addition is 12,000 ~ 16,000 U/L squid prepared Chinese ink supernatants, and neutral proteinase addition is 5,000 ~ 9,
000U/ L squid prepared Chinese ink supernatants, 40 ~ 60 DEG C of hydrolysis temperature, pH value 7 ~ 9,3 ~ 5h of enzyme digestion reaction time；Enzyme digestion reaction starts,
Every 1h with 5 ~ 30min of ultrasound-assisted enzymolysis, ultrasonic sound field intensity is 60W/cm2, supersonic frequency is 20 ~ 25kHz.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110092845A (en) * | 2019-05-07 | 2019-08-06 | 山东大学 | A kind of low molecular weight Sepia polysaccharide and preparation method and application |
| CN112480286A (en) * | 2020-12-01 | 2021-03-12 | 上海市农业科学院 | Method for preparing ganoderma lucidum beta-glucooligosaccharide by degrading ganoderma lucidum beta-glucan |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1895665A (en) * | 2006-06-26 | 2007-01-17 | 宁波超星海洋生物制品有限公司 | Scorpionfish-ink polysaccharide and its preparation |
| CN103304686A (en) * | 2013-06-28 | 2013-09-18 | 江苏大学 | Method for preparing oligomeric narrow-molecular weight distribution chitosan oligosaccharides through ultrasonic-microwave synergetic oxidation |
| CN103936877A (en) * | 2014-04-24 | 2014-07-23 | 湖州康企药业有限公司 | Method for extracting mucopolysaccharides from cuttlefish ink sac |
-
2017
- 2017-09-22 CN CN201710867431.1A patent/CN107793491A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1895665A (en) * | 2006-06-26 | 2007-01-17 | 宁波超星海洋生物制品有限公司 | Scorpionfish-ink polysaccharide and its preparation |
| CN103304686A (en) * | 2013-06-28 | 2013-09-18 | 江苏大学 | Method for preparing oligomeric narrow-molecular weight distribution chitosan oligosaccharides through ultrasonic-microwave synergetic oxidation |
| CN103936877A (en) * | 2014-04-24 | 2014-07-23 | 湖州康企药业有限公司 | Method for extracting mucopolysaccharides from cuttlefish ink sac |
Non-Patent Citations (4)
| Title |
|---|
| CHEN SG ET AL: "Sequence determination of a non-sulfated glycosaminoglycan-like polysaccharide from melanin-free ink of the squid Ommastrephes bartrami by negative-ion electrospray tandem mass spectrometry and NMR spectroscopy", 《GLYCOCONJUGATE JOURNAL》 * |
| TAO ZUO ET AL: "Transportation of squid ink polysaccharide SIP through intestinal epithelial cells and its utilization in the gastrointestinal tract", 《JOURNAL OF FUNCTIONAL FOODS》 * |
| 郭力等: "《中药化学实验》", 31 July 2015, 中国医药科技出版社 * |
| 陈士国: "几种海洋动物酸性多糖的结构和活性研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110092845A (en) * | 2019-05-07 | 2019-08-06 | 山东大学 | A kind of low molecular weight Sepia polysaccharide and preparation method and application |
| CN112480286A (en) * | 2020-12-01 | 2021-03-12 | 上海市农业科学院 | Method for preparing ganoderma lucidum beta-glucooligosaccharide by degrading ganoderma lucidum beta-glucan |
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