CN105661543B - A kind of stable type intestines sustained release tea polyphenols microcapsules and preparation method thereof - Google Patents
A kind of stable type intestines sustained release tea polyphenols microcapsules and preparation method thereof Download PDFInfo
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- CN105661543B CN105661543B CN201610057349.8A CN201610057349A CN105661543B CN 105661543 B CN105661543 B CN 105661543B CN 201610057349 A CN201610057349 A CN 201610057349A CN 105661543 B CN105661543 B CN 105661543B
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- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 209
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 209
- 239000003094 microcapsule Substances 0.000 title claims abstract description 112
- 210000000936 intestine Anatomy 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 241001122767 Theaceae Species 0.000 title claims description 163
- 238000013268 sustained release Methods 0.000 title claims description 17
- 239000012730 sustained-release form Substances 0.000 title claims description 17
- 239000000243 solution Substances 0.000 claims abstract description 71
- 229920001661 Chitosan Polymers 0.000 claims abstract description 34
- 108010010803 Gelatin Proteins 0.000 claims abstract description 28
- 229920000159 gelatin Polymers 0.000 claims abstract description 28
- 239000008273 gelatin Substances 0.000 claims abstract description 28
- 235000019322 gelatine Nutrition 0.000 claims abstract description 28
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 108010073771 Soybean Proteins Proteins 0.000 claims abstract description 24
- 235000019710 soybean protein Nutrition 0.000 claims abstract description 24
- 230000002459 sustained effect Effects 0.000 claims abstract description 22
- 244000068988 Glycine max Species 0.000 claims abstract description 19
- 235000010469 Glycine max Nutrition 0.000 claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- 239000000839 emulsion Substances 0.000 claims abstract description 17
- 101710089165 Protein white Proteins 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 15
- 238000001694 spray drying Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 8
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 2
- 230000003078 antioxidant effect Effects 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 244000269722 Thea sinensis Species 0.000 abstract 4
- 230000007760 free radical scavenging Effects 0.000 description 35
- 239000000463 material Substances 0.000 description 14
- 230000001186 cumulative effect Effects 0.000 description 12
- 230000000968 intestinal effect Effects 0.000 description 12
- 239000012530 fluid Substances 0.000 description 10
- 210000004051 gastric juice Anatomy 0.000 description 10
- 239000002775 capsule Substances 0.000 description 7
- 239000003814 drug Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 150000003254 radicals Chemical class 0.000 description 6
- 239000003292 glue Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000003929 acidic solution Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000012458 free base Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 3
- 235000005487 catechin Nutrition 0.000 description 3
- 229950001002 cianidanol Drugs 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 239000011162 core material Substances 0.000 description 2
- 150000007965 phenolic acids Chemical class 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000012460 protein solution Substances 0.000 description 2
- 235000018102 proteins Nutrition 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 230000003578 releasing effect Effects 0.000 description 2
- 210000002784 stomach Anatomy 0.000 description 2
- LSHVYAFMTMFKBA-TZIWHRDSSA-N (-)-epicatechin-3-O-gallate Chemical compound O([C@@H]1CC2=C(O)C=C(C=C2O[C@@H]1C=1C=C(O)C(O)=CC=1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 LSHVYAFMTMFKBA-TZIWHRDSSA-N 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 102000057297 Pepsin A Human genes 0.000 description 1
- 108090000284 Pepsin A Proteins 0.000 description 1
- 229920002494 Zein Polymers 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229930002878 anthoxanthin Natural products 0.000 description 1
- 150000004637 anthoxanthins Chemical class 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000000675 anti-caries Effects 0.000 description 1
- 230000002019 anti-mutation Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 239000005018 casein Substances 0.000 description 1
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 description 1
- 235000021240 caseins Nutrition 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 235000013601 eggs Nutrition 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003232 mucoadhesive effect Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229940111202 pepsin Drugs 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 229920000747 poly(lactic acid) Polymers 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000005019 zein Substances 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a kind of stable type intestines to be sustained tea polyphenols microcapsules and preparation method thereof, and preparation method is：(1) tea polyphenols solution is prepared；(2) pH value of soybean separation protein white water solution is adjusted；(3) by soybean separation protein white water solution and tea polyphenols solution mixing, mixed liquor is obtained；(4) mixed liquor is mixed with aqueous gelatin solution, is stirred evenly, adjusted pH with HCl/water solution, obtain soybean protein isolate/gelatin emulsion；(5) chitosan will be configured to chitosan solution with acetic acid aqueous solution, soybean protein isolate/gelatin emulsion is mixed with chitosan solution, is stirred evenly, spray drying obtains.The tea polyphenols microcapsules of the present invention are biodegradable, observe spherical in shape under scanning electron microscope, and surface is smooth, without being adhered, no recess.Still there is very high physical stability under strong acid, highly basic, hot conditions and keep good antioxidant activity.The method preparation process of the present invention is easy, nontoxic, safety, and microencapsulation degree is high.
Description
Technical field
The present invention relates to a kind of stable type intestines to be sustained tea polyphenols microcapsules and preparation method thereof, belongs to microencapsulation technology and answers
Use field.
Background technology
Tea polyphenols also known as tea tannin are the general name of polyhydroxyl phenolic compound contained in tealeaves, including catechin
The ingredients such as class, anthocyan, anthoxanthins, phenolic acid and carboxylic phenolic acid class, wherein catechin account for the 65%~80% of polyphenol total amount.
Tea polyphenols have stronger bioactivity and pharmacological activity, there is prevention and cure of cardiovascular disease, anticancer, antimutation, blood pressure lowering, drop blood
The effects that sugar, anti-caries.However, since it is with active polyhydroxy structure, make it under the environment of high temperature, illumination or humidity
It is oxidizable rotten, the bioavilability of tea polyphenols is reduced, the bioactivity of tea polyphenols is made to cannot get maximum performance.
Microcapsule technology is that solid drugs or liquid medicine are rolled into microencapsulation using macromolecule natural or synthetic material.
Microcapsule technology is quickly grown in recent years, is increasingly being applied to the fields such as medicine, biomedicine, food, cosmetics.Using
This technology of micro-capsule can improve medicine stability, mitigate adverse drug smell, be conducive to the production, storage and use of drug.
As that studies tea polyphenols gradually gos deep into, it is intended to improve the research of tea polyphenol stability by preparing micro-capsule
It increasingly reports, but generally speaking, there is also certain shortcoming, examples for the current existing method for preparing tea polyphenols microcapsules
Such as：Lee medicine orchid et al. prepares tea polyphenols microcapsules with ethyl cellulose and polylactic acid respectively, the experimental results showed that, though the former is to tea
Polyphenol has preferable protective effect and encapsulation rate is higher, but the relative amount of its major physiological active constituent catechin reduces；Afterwards
Although person ensure that the relative amount of active ingredient, encapsulation rate, slow release speed are not ideal enough.In addition, with single wall material
The microcapsules prepared can seriously affect the organoleptic feature of microcapsules, be unfavorable in spray-drying process because of acutely dehydration
The embedding of polyphenol.
In recent years, protein is increasingly taken seriously as the wall material of microcapsules, and there are commonly the white eggs of (people or ox) serum
In vain, zein, casein, soybean protein isolate etc., soybean protein isolate is negatively charged more than isoelectric point, can be with acid condition
Under positively charged chitosan electrostatic interaction occur realize microencapsulation to which cohesion is coated on around core material.In addition, mostly
Number albumen reasonable price, raw material are easy to get.In addition, single wall material can be well solved by preparing microcapsules using compound wall materials wall material
Deficiency in terms of certain, achievees the purpose that mutual supplement with each other's advantages, hence it is evident that improves the physical stability of core material and ensures its bioactivity.At present
It has not been found that using soybean protein isolate, gelatin, chitosan prepares the report of tea polyphenols microcapsules as compound wall materials.
Invention content
The problem of being encountered in being prepared for tea polyphenols microcapsules in the prior art, the present invention provides one kind to be detached with soybean
Albumen/gelatin/chitosan is that a kind of stable type intestines of compound wall materials are sustained tea polyphenols microcapsules.
Second object of the present invention is to provide a kind of preparation method of stable type intestines sustained release tea polyphenols microcapsules.
Technical scheme of the present invention is summarized as follows：
A kind of preparation method of stable type intestines sustained release tea polyphenols microcapsules, includes the following steps：
(1) tea polyphenols by purity more than 50% are made into concentration with the ethanol water that volumetric concentration is 75%~99.7%
For the tea polyphenols solution of 1~2mg/mL；
(2) soybean that mass concentration is 12%~20% is detached with the NaOH aqueous solutions of a concentration of 0.1~0.5mol/L
The pH value of protein solution is adjusted to 7~13；
(3) by volume by the soybean separation protein white water solution that step (2) obtains and the tea polyphenols solution that step (1) obtains
1~6:1 ratio is uniformly mixed, and obtains mixed liquor；
(4) it is 100~150 by volume:1 ratio, by mixed liquor and mass percentage be 2%~4.5% it is bright
Glue solution mixes, and is stirred evenly under the conditions of 0~4 DEG C, and pH to 4 is adjusted with the HCl/water solution of a concentration of 0.1~0.5mol/L
~5, obtain soybean protein isolate/gelatin emulsion；
(5) acetic acid aqueous solution for being 1%~5% with volumetric concentration by be 0.25~0.65Pas by viscosity chitosan
It is configured to the chitosan solution of a concentration of 8~12mg/mL, is by volume 1:1~3 ratio is by soybean protein isolate/gelatin
Emulsion is mixed with chitosan solution, is stirred evenly, and spray drying obtains stable type intestines and is sustained tea polyphenols microcapsules.
Step (2) is preferably：The soybean that mass concentration is 15% is detached with the NaOH aqueous solutions of a concentration of 0.3mol/L
The pH value of protein solution is adjusted to 9.
Step (3) is preferably：By the soybean separation protein white water solution that step (2) obtains and the tea polyphenols that step (1) obtains
Solution by volume 2：1 ratio is uniformly mixed, and obtains mixed liquor.
Step (4) is preferably：It is 130 by volume:1 ratio, by mixed liquor and mass percentage be 2.5% it is bright
Glue solution mixes, and is stirred evenly under the conditions of 4 DEG C, adjusts pH to 4.5 with the HCl/water solution of a concentration of 0.3mol/L, obtains
Soybean protein isolate/gelatin emulsion.
Step (5) is preferably：The acetic acid aqueous solution for being 3% with volumetric concentration matches the chitosan that viscosity is 0.45Pas
The chitosan solution of a concentration of 10mg/mL is made, is by volume 1:2 ratio by soybean protein isolate/gelatin emulsion with
Chitosan solution mixes, and stirs evenly, and spray drying obtains stable type intestines and is sustained tea polyphenols microcapsules.
Stable type intestines prepared by the above method are sustained tea polyphenols microcapsules.
Advantages of the present invention：
(1) stable type intestines are prepared present invention employs the spray-dried method of compound wall materials and is sustained tea polyphenols microcapsules, as
The soybean protein isolate and chitosan of natural biological macromolecular have the advantages such as safe and environment-friendly, micro-encapsulation technology is excellent, gelatin
Raw material is easy to get, is cheap, better mechanical property, stable chemical performance and with it is biodegradable many advantages, such as.The present invention
Using chitosan as composite micro-capsule outer layer wall material, good filming ability and the Mucoadhesive for having given full play to chitosan are special
Property, can be colonized in small intestinal mucosal surface, be more suitable for preparing the wall material of intestinal-specific microcapsules, tea polyphenols by oral administration after
The unfavorable conditions in stomach can be avoided, enteron aisle position is reached to maximum, gelatin and soybean under neutral or weak basic condition
Protein isolate dissolves so that tea polyphenols effectively release.
(2) the microcapsule embedded effect that prepared by the present invention is good；Gained microcapsules observe the ball in rule under scanning electron microscope
Shape, surface is smooth, and nothing is adhered, no recess.Organoleptic feature is in smaller particle, preferable mobility and fine and smooth feel.
(3) method preparation process of the invention is easy, nontoxic, and safety, microencapsulation degree is high, gained tea polyphenols microcapsules
Stability is high, and the tea polyphenols microcapsules prepared still have very high physical stability simultaneously under strong acid, highly basic, hot conditions
Keep good antioxidant activity.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph that stable type intestines are sustained tea polyphenols microcapsules.
Fig. 2 is that tea polyphenols and stable type intestines are sustained tea in tea polyphenols microcapsules (abbreviation tea polyphenols microcapsules) after storing 20 days
The changes of contents of polyphenol.
Fig. 3 is that tea polyphenols and stable type intestines are sustained tea in tea polyphenols microcapsules (abbreviation tea polyphenols microcapsules) after storing 20 days
The antioxidant activity of polyphenol changes.
Fig. 4 is pH>The antioxygen of tea polyphenols and stable type intestines sustained release tea polyphenols microcapsules (abbreviation tea polyphenols microcapsules) when 13
Change activity change.
Fig. 5 is pH<Tea polyphenols and stable type intestines are sustained the anti-oxidant of tea polyphenols microcapsules (abbreviation tea polyphenols microcapsules) when 1
Activity change.
Tea polyphenols and stable type intestines are sustained the anti-oxidant of tea polyphenols microcapsules (abbreviation tea polyphenols microcapsules) when Fig. 6 is 90 DEG C
Activity change.
Fig. 7 is that stable type intestines are sustained sustained release situation of the tea polyphenols microcapsules in simulate the gastric juice and simulated intestinal fluid in 30min.
Specific implementation mode
With reference to specific embodiment, the present invention is further illustrated.
Tea polyphenols are commercially available, and purity is more than 50%；
Soybean protein isolate：It is purchased from Beijing extensive and profound in meaning star biotechnology Co., Ltd；
Gelatin：It is purchased from Tianjin sky over the river Chemical Engineering Technology Co., Ltd；
Chitosan：It is purchased from ZHEJIANG AOXING BIOTECHNOLOGY CO., LTD；
Pepsin：It is purchased from hundred times of Tianjin bio tech ltd；
Trypsase：It is purchased from hundred times of Tianjin bio tech ltd；
1,1- diphenyl picryl phenylhydrazines (DPPH)：It is purchased from Sigma Co., USA；
The introduction of above-mentioned raw materials is in order to enable those skilled in the art to more fully understand the present invention, but not to this
Invention imposes any restrictions, and all raw materials similar with above-mentioned raw materials may be used to the present invention.
Specific embodiment
By following embodiment, the invention will be further described, it is not limited in following embodiment and embodiment
Process parameters range.Wherein polyphenol content is measured using national standard GB/T 8313-2002 methods.
Embodiment 1
A kind of stable type intestines sustained release tea polyphenols microcapsules and preparation method thereof, include the following steps：
(1) tea polyphenols that purity is 98.0% are made into a concentration of 1mg/mL with the ethanol water that volumetric concentration is 80%
Tea polyphenols solution；
(2) the soybean separation protein white water solution for being 15% by mass concentration with the NaOH aqueous solutions of a concentration of 0.3mol/L
PH value is adjusted to 9；
(3) by volume by the soybean separation protein white water solution that step (2) obtains and the tea polyphenols solution that step (1) obtains
2：1 ratio is uniformly mixed, and obtains mixed liquor；
(4) it is 130 by volume:1 ratio mixes the aqueous gelatin solution that mixed liquor is 2.5% with mass percentage
Close, stir evenly under the conditions of 4 DEG C, pH to 4.5 is adjusted with the HCl/water solution of a concentration of 0.3mol/L, obtain soybean protein isolate/
Gelatin emulsion；
(5) chitosan that viscosity is 0.45Pas is configured to a concentration of by the acetic acid aqueous solution for being 3% with volumetric concentration
The chitosan solution of 10mg/mL is by volume 1:2 ratio is mixed soybean protein isolate/gelatin emulsion and chitosan
Solution mixes, and stirs evenly, and spray drying obtains stable type intestines and is sustained tea polyphenols microcapsules.
After being placed at room temperature for 20 days, the polyphenol content damage in the tea polyphenols (hereinafter referred to as tea polyphenols) that material purity is 98.0%
43.18% is lost, the polyphenol content in stable type intestines sustained release tea polyphenols microcapsules (hereinafter referred to as tea polyphenols microcapsules) has lost
6.98%.Compared with tea polyphenols, the polyphenol content loss in tea polyphenols microcapsules is less, sees Fig. 2.
After being placed at room temperature for 20 days, the DPPH free radical scavenging activities of tea polyphenols drop to 80.45% by 98% before, and tea is more
The DPPH free radical scavenging activities of phenol microcapsules remain at 97%.Compared with tea polyphenols, the DPPH free radicals of tea polyphenols microcapsules
Clearance rate declines unobvious, sees Fig. 3.
Tea polyphenols and tea polyphenols microcapsules are placed on pH>1h is acted in 13 strong alkali solution, the DPPH of the two is free
Base clearance rate is declined, and the DPPH free radical scavenging activities of tea polyphenols drop to 18.67% by 95.43% before, and tea
Though the DPPH free radical scavenging activities of polyphenol microcapsules have reduction, but still can reach 67.20%, Fig. 4 is seen.
Tea polyphenols and tea polyphenols microcapsules are placed on pH<1h, the DPPH free radicals of the two are acted in 1 strongly acidic solution
Clearance rate is declined, and the DPPH free radical scavenging activities of tea polyphenols drop to 75% by 95.38% before, and tea polyphenols are micro-
The DPPH free radical scavenging activities of capsule slightly reduce, and still can reach 90.12%, see Fig. 5.
Tea polyphenols and tea polyphenols microcapsules are placed into 2h in 90 DEG C of environment, the DPPH free radical scavenging activities of the two are
Declining, the DPPH free radical scavenging activities of tea polyphenols drop to 63.56% by 95.73% before, and tea polyphenols microcapsules
DPPH free radical scavenging activities slightly reduce, and still can reach 87.65%, see Fig. 6.
Tea polyphenols microcapsules are individually positioned in simulate the gastric juice and simulated intestinal fluid and are digested, it is micro- to calculate tea polyphenols in 30min
The cumulative release amount of polyphenol in capsule, the experimental results showed that, the tea polyphenols in tea polyphenols microcapsules discharged in simulate the gastric juice compared with
Few, the cumulative release amount in 30min is 25.18%, and is discharged in simulated intestinal fluid more, and the cumulative release amount in 30min can
To reach 87.23%, Fig. 7 is seen.
Embodiment 2
A kind of stable type intestines sustained release tea polyphenols microcapsules and preparation method thereof, include the following steps：
(1) tea polyphenols that purity is 98.23% are made into a concentration of 2mg/ with the ethanol water that volumetric concentration is 75%
The tea polyphenols solution of mL；
(2) the soybean separation protein white water solution for being 12% by mass concentration with the NaOH aqueous solutions of a concentration of 0.1mol/L
PH value is adjusted to 7；
(3) by volume by the soybean separation protein white water solution that step (2) obtains and the tea polyphenols solution that step (1) obtains
1：1 ratio is uniformly mixed, and obtains mixed liquor；
(4) it is 100 by volume:1 ratio mixes mixed liquor with the aqueous gelatin solution that mass percentage is 2%,
It is stirred evenly under the conditions of 0 DEG C, adjusts pH to 4 with the HCl/water solution of a concentration of 0.1mol/L, obtain soybean protein isolate/gelatin
Emulsion；
(5) chitosan that viscosity is 0.25Pas is configured to a concentration of by the acetic acid aqueous solution for being 1% with volumetric concentration
The chitosan solution of 8mg/mL is by volume 1:1 ratio mixes soybean protein isolate/gelatin emulsion with chitosan solution
It closes, stirs evenly, spray drying obtains stable type intestines and is sustained tea polyphenols microcapsules.
After being placed at room temperature for 20 days, the polyphenol content in the tea polyphenols (hereinafter referred to as tea polyphenols) that material purity is 98.23%
45.25% is had lost, stable type intestines are sustained the polyphenol content loss in tea polyphenols microcapsules (hereinafter referred to as tea polyphenols microcapsules)
6.46%.Compared with tea polyphenols, the polyphenol content loss in tea polyphenols microcapsules is less, sees Fig. 2.
After being placed at room temperature for 20 days, the DPPH free radical scavenging activities of tea polyphenols drop to 78.93% by 97.64% before,
The DPPH free radical scavenging activities of tea polyphenols microcapsules remain at 96.88%.Compared with tea polyphenols, the DPPH of tea polyphenols microcapsules
Free radical scavenging activity declines unobvious, sees Fig. 3.
Tea polyphenols and tea polyphenols microcapsules are placed on pH>1h is acted in 13 strong alkali solution, the DPPH of the two is free
Base clearance rate is declined, and the DPPH free radical scavenging activities of tea polyphenols drop to 18.23% by 95.37% before, and tea
Though the DPPH free radical scavenging activities of polyphenol microcapsules have reduction, but still can reach 63.17%, Fig. 4 is seen.
Tea polyphenols and tea polyphenols microcapsules are placed on pH<1h, the DPPH free radicals of the two are acted in 1 strongly acidic solution
Clearance rate is declined, and the DPPH free radical scavenging activities of tea polyphenols drop to 74.80% by 95.39% before, and tea is more
The DPPH free radical scavenging activities of phenol microcapsules slightly reduce, and still can reach 92%, see Fig. 5.
Tea polyphenols and tea polyphenols microcapsules are placed into 2h in 90 DEG C of environment, the DPPH free radical scavenging activities of the two are
Declining, the DPPH free radical scavenging activities of tea polyphenols drop to 65.28% by 95.68% before, and tea polyphenols microcapsules
DPPH free radical scavenging activities slightly reduce, and still can reach 83.11%, see Fig. 6.
Tea polyphenols microcapsules are individually positioned in simulate the gastric juice and simulated intestinal fluid and are digested, it is micro- to calculate tea polyphenols in 30min
The cumulative release amount of polyphenol in capsule, the experimental results showed that, the polyphenol in tea polyphenols microcapsules discharged in simulate the gastric juice it is less,
Cumulative release amount in 30min is 24.29%, and is discharged in simulated intestinal fluid more, and the cumulative release amount in 30min can reach
To 84.26%, Fig. 7 is seen.
Embodiment 3
A kind of stable type intestines sustained release tea polyphenols microcapsules and preparation method thereof, include the following steps：
(1) tea polyphenols that purity is 98.18% are made into the ethanol water that volumetric concentration is 99.7% a concentration of
The tea polyphenols solution of 1.2mg/mL；
(2) the soybean separation protein white water solution for being 18% by mass concentration with the NaOH aqueous solutions of a concentration of 0.4mol/L
PH value is adjusted to 11；
(3) by volume by the soybean separation protein white water solution that step (2) obtains and the tea polyphenols solution that step (1) obtains
4：1 ratio is uniformly mixed, and obtains mixed liquor；
(4) it is 125 by volume:1 ratio mixes mixed liquor with the aqueous gelatin solution that mass percentage is 3%,
It is stirred evenly under the conditions of 2 DEG C, pH to 4.7 is adjusted with the HCl/water solution of a concentration of 0.4mol/L, obtain soybean protein isolate/bright
Glue emulsion；
(5) chitosan that viscosity is 0.3Pas is configured to a concentration of by the acetic acid aqueous solution for being 2.5% with volumetric concentration
The chitosan solution of 9mg/mL is by volume 1:2.5 ratio is by soybean protein isolate/gelatin emulsion and chitosan solution
Mixing, stirs evenly, and spray drying obtains stable type intestines and is sustained tea polyphenols microcapsules.
After being placed at room temperature for 20 days, the polyphenol content in the tea polyphenols (hereinafter referred to as tea polyphenols) that material purity is 98.18%
42.88% is had lost, stable type intestines are sustained the polyphenol content loss in tea polyphenols microcapsules (hereinafter referred to as tea polyphenols microcapsules)
7.16%.Compared with tea polyphenols, the polyphenol content loss in tea polyphenols microcapsules is less, sees Fig. 2.
After being placed at room temperature for 20 days, the DPPH free radical scavenging activities of tea polyphenols drop to 76.93% by 98.86% before,
The DPPH free radical scavenging activities of tea polyphenols microcapsules remain at 95.23%.Compared with tea polyphenols, the DPPH of tea polyphenols microcapsules
Free radical scavenging activity declines unobvious, sees Fig. 3.
Tea polyphenols and tea polyphenols microcapsules are placed on pH>1h is acted in 13 strong alkali solution, the DPPH of the two is free
Base clearance rate is declined, and the DPPH free radical scavenging activities of tea polyphenols drop to 16.20% by 96.75% before, and tea
Though the DPPH free radical scavenging activities of polyphenol microcapsules have reduction, but still can reach 62.39%, Fig. 4 is seen.
Tea polyphenols and tea polyphenols microcapsules are placed on pH<1h, the DPPH free radicals of the two are acted in 1 strongly acidic solution
Clearance rate is declined, and the DPPH free radical scavenging activities of tea polyphenols drop to 73% by 95.41% before, and tea polyphenols are micro-
The DPPH free radical scavenging activities of capsule slightly reduce, and still can reach 94.32%, see Fig. 5.
Tea polyphenols and tea polyphenols microcapsules are placed into 2h in 90 DEG C of environment, the DPPH free radical scavenging activities of the two are
Declining, the DPPH free radical scavenging activities of tea polyphenols drop to 64.30% by 96.03% before, and tea polyphenols microcapsules
DPPH clearance rates slightly reduce, and still can reach 86.19%, see Fig. 6.
Tea polyphenols microcapsules are individually positioned in simulate the gastric juice and simulated intestinal fluid and are digested, it is micro- to calculate tea polyphenols in 30min
The cumulative release amount of polyphenol in capsule, the experimental results showed that, the polyphenol in tea polyphenols microcapsules discharged in simulate the gastric juice it is less,
Cumulative release amount in 30min is 23.96%, and is discharged in simulated intestinal fluid more, and the cumulative release amount in 30min can reach
To 86.73%, Fig. 7 is seen.
Embodiment 4
A kind of stable type intestines sustained release tea polyphenols microcapsules and preparation method thereof, include the following steps：
(1) tea polyphenols that purity is 98.42% are made into the ethanol water that volumetric concentration is 85% a concentration of
The tea polyphenols solution of 1.5mg/mL；
(2) the soybean separation protein white water solution for being 20% by mass concentration with the NaOH aqueous solutions of a concentration of 0.5mol/L
PH value is adjusted to 13；
(3) by volume by the soybean separation protein white water solution that step (2) obtains and the tea polyphenols solution that step (1) obtains
6：1 ratio is uniformly mixed, and obtains mixed liquor；
(4) it is 150 by volume:1 ratio mixes the aqueous gelatin solution that mixed liquor is 4.5% with mass percentage
It closes, stirs evenly under the conditions of 1 DEG C, pH to 5 is adjusted with the HCl/water solution of a concentration of 0.5mol/L, obtain soybean protein isolate/bright
Glue emulsion；
(5) chitosan that viscosity is 0.65Pas is configured to a concentration of by the acetic acid aqueous solution for being 5% with volumetric concentration
The chitosan solution of 12mg/mL is by volume 1:3 ratio is by soybean protein isolate/gelatin emulsion and chitosan solution
Mixing, stirs evenly, and spray drying obtains stable type intestines and is sustained tea polyphenols microcapsules.
After being placed at room temperature for 20 days, the polyphenol content damage for the tea polyphenols (hereinafter referred to as tea polyphenols) that material purity is 98.42%
44.12% is lost, the polyphenol content in stable type intestines sustained release tea polyphenols microcapsules (hereinafter referred to as tea polyphenols microcapsules) has lost
7.45%.Compared with tea polyphenols, the polyphenol content loss in tea polyphenols microcapsules is less, sees Fig. 2.
After being placed at room temperature for 20 days, the DPPH free radical scavenging activities of tea polyphenols drop to 78.90% by 98.21% before,
The DPPH free radical scavenging activities of tea polyphenols microcapsules remain at 98%.Compared with tea polyphenols, the DPPH of tea polyphenols microcapsules is certainly
Unobvious are declined by base clearance rate, see Fig. 3.
Tea polyphenols and tea polyphenols microcapsules are placed on pH>1h is acted in 13 strong alkali solution, the DPPH of the two is free
Base clearance rate is declined, and the DPPH free radicals rates of tea polyphenols drops to 17.56% by 97% before, and the micro- glue of tea polyphenols
Though the DPPH free radical scavenging activities of capsule have reduction, but still can reach 65.12%, Fig. 4 is seen.
Tea polyphenols and tea polyphenols microcapsules are placed on pH<1h, the DPPH free radicals of the two are acted in 1 strongly acidic solution
Clearance rate is declined, and the DPPH free radical scavenging activities of tea polyphenols drop to 76.11% by 97.06% before, and tea is more
The DPPH free radical scavenging activities of phenol microcapsules slightly reduce, and still can reach 93.46%, see Fig. 5.
Tea polyphenols and tea polyphenols microcapsules are placed into 2h in 90 DEG C of environment, the DPPH free radical scavenging activities of the two are
Declining, the DPPH free radical scavenging activities of tea polyphenols drop to 69.73% by 95.44% before, and tea polyphenols microcapsules
DPPH clearance rates slightly reduce, and still can reach 85.66%, see Fig. 6.
Tea polyphenols microcapsules are individually positioned in simulate the gastric juice and simulated intestinal fluid and are digested, it is micro- to calculate tea polyphenols in 30min
The cumulative release amount of polyphenol in capsule, the experimental results showed that, the polyphenol in tea polyphenols microcapsules discharged in simulate the gastric juice it is less,
Cumulative release amount in 30min is 24.78%, and is discharged in simulated intestinal fluid more, and the cumulative release amount in 30min can reach
To 85.87%, Fig. 7 is seen.
Electron-microscope scanning is carried out to the stable delayed tea polyphenols microcapsules that embodiment 1 obtains, Fig. 1 is seen, observes microcapsules
Package status.Tea polyphenols microcapsules amplify 600 times of observations under a scanning electron microscope, and appearance is very complete, in relatively regular
Spherical shape, surface is smooth, and nothing is adhered, pucker-free, no recess, and grain size is concentrated mainly on 10~200 μm, and embedding effect is preferable.
The tea polyphenols microcapsule stability that the present invention prepares it can be seen from each embodiment result is very high, strong
Good antioxidant activity is still kept under acid, highly basic, hot conditions, burst size of the microcapsules in simulated intestinal fluid is relatively high, and
Burst size in simulate the gastric juice is relatively low, effectively avoids highly acidity environment in tea polyphenols contact stomach and is destroyed, has enteron aisle
Slow-releasing and controlled-releasing action.
Claims (6)
1. a kind of preparation method of stable type intestines sustained release tea polyphenols microcapsules, it is characterized in that including the following steps：
(1) tea polyphenols by purity more than 50% are made into a concentration of 1 with the ethanol water that volumetric concentration is 75%~99.7%
The tea polyphenols solution of~2mg/mL；
(2) soybean protein isolate for being 12%~20% by mass concentration with the NaOH aqueous solutions of a concentration of 0.1~0.5mol/L
The pH value of aqueous solution is adjusted to 7~13；
(3) by the soybean separation protein white water solution that step (2) obtains and the tea polyphenols solution that step (1) obtains by volume 1~
6:1 ratio is uniformly mixed, and obtains mixed liquor；
(4) it is 100~150 by volume:1 ratio, the gelatin water for being 2%~4.5% by mixed liquor and mass percentage
Solution mixes, and is stirred evenly under the conditions of 0~4 DEG C, and pH to 4~5 is adjusted with the HCl/water solution of a concentration of 0.1~0.5mol/L,
Obtain soybean protein isolate/gelatin emulsion；
(5) acetic acid aqueous solution for being 1%~5% with volumetric concentration prepares the chitosan for being 0.25~0.65Pas by viscosity
It is by volume 1 at the chitosan solution of a concentration of 8~12mg/mL:1~3 ratio is by soybean protein isolate/gelatin emulsus
Liquid is mixed with chitosan solution, is stirred evenly, and spray drying obtains stable type intestines and is sustained tea polyphenols microcapsules.
2. a kind of preparation method of stable type intestines sustained release tea polyphenols microcapsules according to claim 1, it is characterised in that step
Suddenly (2) are：With the pH for the soybean separation protein white water solution that mass concentration is 15% by the NaOH aqueous solutions of a concentration of 0.3mol/L
Value is adjusted to 9.
3. a kind of preparation method of stable type intestines sustained release tea polyphenols microcapsules according to claim 1, it is characterised in that step
Suddenly (3) are：By the soybean separation protein white water solution that step (2) obtains and the tea polyphenols solution that step (1) obtains by volume 2：1
Ratio be uniformly mixed, obtain mixed liquor.
4. a kind of preparation method of stable type intestines sustained release tea polyphenols microcapsules according to claim 1, it is characterised in that step
Suddenly (4) are：It is 130 by volume:1 ratio mixes mixed liquor with the aqueous gelatin solution that mass percentage is 2.5%,
Stirred evenly under the conditions of 4 DEG C, pH to 4.5 adjusted with the HCl/water solution of a concentration of 0.3mol/L, obtain soybean protein isolate/
Gelatin emulsion.
5. a kind of preparation method of stable type intestines sustained release tea polyphenols microcapsules according to claim 1, it is characterised in that step
Suddenly (5) are：The chitosan that viscosity is 0.45Pas is configured to a concentration of 10mg/ by the acetic acid aqueous solution for being 3% with volumetric concentration
The chitosan solution of mL is by volume 1:2 ratio mixes soybean protein isolate/gelatin emulsion with chitosan solution,
It stirs evenly, spray drying obtains stable type intestines and is sustained tea polyphenols microcapsules.
6. stable type intestines prepared by the method for claim 1-5 any one are sustained tea polyphenols microcapsules.
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| CN106509899A (en) * | 2016-11-15 | 2017-03-22 | 江南大学 | Method for compounding and entrapping tea polyphenols through debranched starch and xanthan gum |
| CN107319549A (en) * | 2017-06-08 | 2017-11-07 | 江苏华冠生物技术股份有限公司 | A kind of microcapsule method for protecting Tea Polyphenols tolerance gut flora to degrade |
| CN107638333A (en) * | 2017-09-29 | 2018-01-30 | 点铂医疗科技（常州）有限公司 | A kind of Tea Polyphenols/chitosan particle and preparation method thereof |
| CN108727836A (en) * | 2018-06-11 | 2018-11-02 | 海南大学 | A kind of preparation method with the edible biogelatin film for being sustained EGCG performances |
| CN111528270A (en) * | 2020-05-28 | 2020-08-14 | 西南科技大学 | Meat product antioxidant tea polyphenol microcapsule and preparation method thereof |
| CN111991368B (en) * | 2020-09-11 | 2021-11-12 | 中国药科大学 | Preparation method of tea polyphenol coated soy protein isolate-quaternary ammonium salt chitosan microcapsule |
| CN112675152A (en) * | 2020-12-25 | 2021-04-20 | 厦门金达威生物科技有限公司 | NMN slow-release enteric-coated microcapsule and preparation method thereof |
| CN115068447B (en) * | 2022-05-13 | 2023-10-20 | 浙江工商大学 | Preparation method of rutin microcapsule |
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