CN115669761B - Microcapsule powder containing tea extract and preparation method and application thereof - Google Patents
Microcapsule powder containing tea extract and preparation method and application thereof Download PDFInfo
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- CN115669761B CN115669761B CN202211235150.1A CN202211235150A CN115669761B CN 115669761 B CN115669761 B CN 115669761B CN 202211235150 A CN202211235150 A CN 202211235150A CN 115669761 B CN115669761 B CN 115669761B
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- microcapsule powder
- tea
- cyclodextrin
- tricalcium phosphate
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- 241001122767 Theaceae Species 0.000 title claims abstract description 70
- 239000000843 powder Substances 0.000 title claims abstract description 57
- 239000003094 microcapsule Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 52
- 238000000605 extraction Methods 0.000 title description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 63
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical class OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 49
- 239000002105 nanoparticle Substances 0.000 claims abstract description 24
- 239000000839 emulsion Substances 0.000 claims abstract description 23
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 10
- 239000001506 calcium phosphate Substances 0.000 claims description 54
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 54
- 229940078499 tricalcium phosphate Drugs 0.000 claims description 54
- 229910000391 tricalcium phosphate Inorganic materials 0.000 claims description 54
- 235000019731 tricalcium phosphate Nutrition 0.000 claims description 54
- 238000002156 mixing Methods 0.000 claims description 41
- 238000003756 stirring Methods 0.000 claims description 34
- 238000005406 washing Methods 0.000 claims description 30
- 229920001661 Chitosan Polymers 0.000 claims description 25
- 239000003607 modifier Substances 0.000 claims description 25
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- 238000010008 shearing Methods 0.000 claims description 21
- 235000013361 beverage Nutrition 0.000 claims description 19
- 229920000858 Cyclodextrin Polymers 0.000 claims description 18
- 239000001116 FEMA 4028 Substances 0.000 claims description 18
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 18
- 229960004853 betadex Drugs 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 13
- 239000012530 fluid Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 9
- 229940092665 tea leaf extract Drugs 0.000 claims description 9
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 8
- 235000012970 cakes Nutrition 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 8
- 235000013365 dairy product Nutrition 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000007710 freezing Methods 0.000 claims description 8
- 230000008014 freezing Effects 0.000 claims description 8
- 125000005456 glyceride group Chemical group 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000002715 modification method Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 8
- 238000004537 pulping Methods 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 235000010413 sodium alginate Nutrition 0.000 claims description 8
- 239000000661 sodium alginate Substances 0.000 claims description 8
- 229940005550 sodium alginate Drugs 0.000 claims description 8
- 239000001509 sodium citrate Substances 0.000 claims description 8
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 8
- 239000000796 flavoring agent Substances 0.000 abstract description 9
- 235000019634 flavors Nutrition 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 6
- 239000004615 ingredient Substances 0.000 abstract description 4
- 238000011156 evaluation Methods 0.000 abstract description 2
- 235000016709 nutrition Nutrition 0.000 abstract description 2
- 238000002386 leaching Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 43
- 239000003921 oil Substances 0.000 description 34
- 230000000052 comparative effect Effects 0.000 description 10
- 235000015243 ice cream Nutrition 0.000 description 7
- 238000012360 testing method Methods 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000012296 anti-solvent Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 150000008442 polyphenolic compounds Chemical class 0.000 description 3
- 235000013824 polyphenols Nutrition 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- JSNRRGGBADWTMC-UHFFFAOYSA-N (6E)-7,11-dimethyl-3-methylene-1,6,10-dodecatriene Chemical compound CC(C)=CCCC(C)=CCCC(=C)C=C JSNRRGGBADWTMC-UHFFFAOYSA-N 0.000 description 2
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- FQTLCLSUCSAZDY-UHFFFAOYSA-N (+) E(S) nerolidol Natural products CC(C)=CCCC(C)=CCCC(C)(O)C=C FQTLCLSUCSAZDY-UHFFFAOYSA-N 0.000 description 1
- 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 1
- CXENHBSYCFFKJS-UHFFFAOYSA-N (3E,6E)-3,7,11-Trimethyl-1,3,6,10-dodecatetraene Natural products CC(C)=CCCC(C)=CCC=C(C)C=C CXENHBSYCFFKJS-UHFFFAOYSA-N 0.000 description 1
- 239000001707 (E,7R,11R)-3,7,11,15-tetramethylhexadec-2-en-1-ol Substances 0.000 description 1
- 239000004386 Erythritol Substances 0.000 description 1
- UNXHWFMMPAWVPI-UHFFFAOYSA-N Erythritol Natural products OCC(O)C(O)CO UNXHWFMMPAWVPI-UHFFFAOYSA-N 0.000 description 1
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 1
- 108010028554 LDL Cholesterol Proteins 0.000 description 1
- FQTLCLSUCSAZDY-ATGUSINASA-N Nerolidol Chemical compound CC(C)=CCC\C(C)=C\CC[C@](C)(O)C=C FQTLCLSUCSAZDY-ATGUSINASA-N 0.000 description 1
- BLUHKGOSFDHHGX-UHFFFAOYSA-N Phytol Natural products CC(C)CCCC(C)CCCC(C)CCCC(C)C=CO BLUHKGOSFDHHGX-UHFFFAOYSA-N 0.000 description 1
- HNZBNQYXWOLKBA-UHFFFAOYSA-N Tetrahydrofarnesol Natural products CC(C)CCCC(C)CCCC(C)=CCO HNZBNQYXWOLKBA-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- BOTWFXYSPFMFNR-OALUTQOASA-N all-rac-phytol Natural products CC(C)CCC[C@H](C)CCC[C@H](C)CCCC(C)=CCO BOTWFXYSPFMFNR-OALUTQOASA-N 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000010692 aromatic oil Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229960001948 caffeine Drugs 0.000 description 1
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 1
- 235000005487 catechin Nutrition 0.000 description 1
- 229950001002 cianidanol Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000010336 energy treatment Methods 0.000 description 1
- UNXHWFMMPAWVPI-ZXZARUISSA-N erythritol Chemical compound OC[C@H](O)[C@H](O)CO UNXHWFMMPAWVPI-ZXZARUISSA-N 0.000 description 1
- 229940009714 erythritol Drugs 0.000 description 1
- 235000019414 erythritol Nutrition 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229930009668 farnesene Natural products 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000000055 hyoplipidemic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- WASNIKZYIWZQIP-AWEZNQCLSA-N nerolidol Natural products CC(=CCCC(=CCC[C@@H](O)C=C)C)C WASNIKZYIWZQIP-AWEZNQCLSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- BOTWFXYSPFMFNR-PYDDKJGSSA-N phytol Chemical compound CC(C)CCC[C@@H](C)CCC[C@@H](C)CCC\C(C)=C\CO BOTWFXYSPFMFNR-PYDDKJGSSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 230000003845 vascular endothelial function Effects 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
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Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Tea And Coffee (AREA)
Abstract
The invention discloses a preparation method of microcapsule powder containing tea extract, which comprises the following steps: adding the oil phase prepared in the second step into the water phase prepared in the third step to obtain a premix; the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder. The microcapsule powder containing the tea extract is prepared by performing supercritical extraction on tea, leaching nutritional ingredients and aroma ingredients of the tea to the greatest extent, taking the tea as an oil phase, performing water phase treatment on the tea by using nanoparticle modified beta-cyclodextrin, performing premixing to form emulsion, and performing treatment by using a supercritical preparation technology, so that the microcapsule powder has excellent stability and retains the original flavor of the tea to the greatest extent; meanwhile, after subjective evaluation of the flavor, the product provided by the invention has excellent mouthfeel, is suitable for being favored by consumers, and has excellent market effect.
Description
Technical Field
The invention relates to the technical field of microcapsule powder, in particular to microcapsule powder containing tea extract and a preparation method and application thereof.
Background
The supercritical fluid granule technology is an emerging technology for preparing target substance fine granules by taking supercritical fluid as a solvent or an anti-solvent and performing a series of physical reactions. Compared with the traditional granulating method (such as an emulsion evaporation method, a spray drying method, a grinding method and a freeze drying method), the supercritical fluid granulating technology does not need high-energy treatment such as shearing, homogenization and the like, does not need to use high temperature to dissolve a sample, and the prepared particles have small and uniform particle size, so that the problems of low yield, non-uniformity, poor activity and the like of the preparation of the fine particles by the traditional method are solved to a great extent. The Supercritical Fluid Emulsion Extraction (SFEE) method is a combination of the traditional emulsification precipitation method and the supercritical antisolvent method, can prepare particles with smaller particle size than the antisolvent method (SAS), and can greatly relieve the problem of particle aggregation.
The tea extract is an active ingredient extracted from tea leaf, and mainly comprises tea polyphenols (catechin), caffeine, aromatic oil, water, minerals, pigments, carbohydrates, proteins, amino acids, vitamins, etc.; the tea polyphenol has the functions of resisting oxidation, scavenging free radicals and the like, obviously reduces the contents of serum total cholesterol, triglyceride and low-density lipoprotein cholesterol of hyperlipidemia, and simultaneously has the functions of recovering and protecting vascular endothelial functions. The hypolipidemic effect of tea polyphenols is also one of the main reasons why tea leaves can make obese people lose weight without rebound.
The existing microcapsule powder can not well preserve aroma components in tea, and tea aroma is easy to burst, so that stability of the tea aroma is affected, and use effect of the microcapsule powder is limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide microcapsule powder containing tea extract, and a preparation method and application thereof, so as to solve the problems in the background art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a preparation method of microcapsule powder containing tea extract, which comprises the following steps:
step one: washing tea leaves with water, draining, freezing in liquid nitrogen, crushing, and performing supercritical extraction to obtain tea leaf extract;
step two: mixing the tea extract with caprylic/capric glyceride according to a weight ratio of 1:5 to form an oil phase;
step three: adding the nanoparticle modified beta-cyclodextrin into 3-6 times of water to form a water phase;
step four: heating the oil phase prepared in the second step to 50-70 ℃, then adding the oil phase into the water phase prepared in the third step, shearing and homogenizing the oil phase to 10000-20000r/min, shearing and homogenizing the oil phase for 25-35min to obtain a premix emulsion;
step five: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
Preferably, the nanoparticle modified beta-cyclodextrin modification method comprises the following steps:
s101: peeling rhizoma Dioscoreae, pulping in 3 times of water, filtering to obtain filtrate, adding 5-10% sodium alginate, and stirring to obtain rhizoma Dioscoreae extractive solution;
s102: adding chitosan into acetic acid to prepare a chitosan solution with the mass fraction of 5%, and then mixing the chitosan solution and the yam extracting solution according to the weight ratio of 5:1 to obtain a modified solution;
s103: adding beta-cyclodextrin into 20-30% of nano tricalcium phosphate modifier, stirring and mixing thoroughly to obtain nano tricalcium phosphate composite beta-cyclodextrin;
s104: s103, mixing the product and the modifying liquid according to the weight ratio of 1: (5-7), stirring and reacting for 20-30min at 60-85 ℃, and washing and drying after stirring to obtain the modified beta-cyclodextrin.
Preferably, the preparation method of the nano tricalcium phosphate modifier comprises the following steps: 10-20 parts of nano tricalcium phosphate is sent into 15-25 parts of hydrochloric acid solution with the mass fraction of 2%, 1-5 parts of CMC-Na and 1-3 parts of sodium citrate are added, stirred and mixed fully, and then water washing and drying are carried out, thus obtaining the nano tricalcium phosphate modifier.
Preferably, the particle size of the nano tricalcium phosphate is 10-30nm.
Preferably, the supercritical preparation technology comprises the following specific operation steps:
injecting the premixed emulsion into a carbon dioxide fluid reaction kettle at 300-330K and 9-12MPa under CO 2 Treating for 30-60min under the condition of flow velocity to obtain suspension;
and (5) washing the suspension for multiple times by using distilled water, and freeze-drying to obtain microcapsule powder.
Preferably, the CO 2 The flow rate is 0.4-0.7L/min.
The invention also provides the tea extract prepared by the preparation method of the microcapsule powder containing the tea extract.
The invention also provides application of the microcapsule powder in beverages, ice cream, cakes and dairy foods.
Compared with the prior art, the invention has the following beneficial effects:
the microcapsule powder containing the tea extract adopts the tea to carry out supercritical extraction, so that the nutritional ingredients and the aroma ingredients of the tea can be leached out to the greatest extent, the tea is used as an oil phase, then the water phase treatment is carried out through nanoparticle modified beta-cyclodextrin, emulsion is formed through premixing, and finally the treatment is carried out through a supercritical preparation technology, so that the microcapsule powder has excellent stability and the original flavor of the tea is retained to the greatest extent; meanwhile, after subjective evaluation of the flavor, the product provided by the invention has excellent mouthfeel, is suitable for being favored by consumers, and has excellent market effect.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a preparation method of microcapsule powder containing tea extract, which comprises the following steps:
step one: washing tea leaves with water, draining, freezing in liquid nitrogen, crushing, and performing supercritical extraction to obtain tea leaf extract;
step two: mixing the tea extract with caprylic/capric glyceride according to a weight ratio of 1:5 to form an oil phase;
step three: adding the nanoparticle modified beta-cyclodextrin into 3-6 times of water to form a water phase;
step four: heating the oil phase prepared in the second step to 50-70 ℃, then adding the oil phase into the water phase prepared in the third step, shearing and homogenizing the oil phase to 10000-20000r/min, shearing and homogenizing the oil phase for 25-35min to obtain a premix emulsion;
step five: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
The modification method of the nanoparticle modified beta-cyclodextrin comprises the following steps:
s101: peeling rhizoma Dioscoreae, pulping in 3 times of water, filtering to obtain filtrate, adding 5-10% sodium alginate, and stirring to obtain rhizoma Dioscoreae extractive solution;
s102: adding chitosan into acetic acid to prepare a chitosan solution with the mass fraction of 5%, and then mixing the chitosan solution and the yam extracting solution according to the weight ratio of 5:1 to obtain a modified solution;
s103: adding beta-cyclodextrin into 20-30% of nano tricalcium phosphate modifier, stirring and mixing thoroughly to obtain nano tricalcium phosphate composite beta-cyclodextrin;
s104: s103, mixing the product and the modifying liquid according to the weight ratio of 1: (5-7), stirring and reacting for 20-30min at 60-85 ℃, and washing and drying after stirring to obtain the modified beta-cyclodextrin.
The preparation method of the nano tricalcium phosphate modifier in the embodiment comprises the following steps: 10-20 parts of nano tricalcium phosphate is sent into 15-25 parts of hydrochloric acid solution with the mass fraction of 2%, 1-5 parts of CMC-Na and 1-3 parts of sodium citrate are added, stirred and mixed fully, and then water washing and drying are carried out, thus obtaining the nano tricalcium phosphate modifier.
The particle size of the nano tricalcium phosphate of the embodiment is 10-30nm.
The specific operation steps of the supercritical preparation technology of the embodiment are as follows:
injecting the premixed emulsion into a carbon dioxide fluid reaction kettle at 300-330K and 9-12MPa under CO 2 Treating for 30-60min under the condition of flow velocity to obtain suspension;
and (5) washing the suspension for multiple times by using distilled water, and freeze-drying to obtain microcapsule powder.
CO of the present embodiment 2 The flow rate is 0.4-0.7L/min.
The tea extract prepared by the preparation method of the microcapsule powder containing the tea extract is provided.
The microcapsule powder is applied to beverages, ice cream, cakes and dairy foods.
Example 1.
The invention provides a preparation method of microcapsule powder containing tea extract, which comprises the following steps:
step one: washing tea leaves with water, draining, freezing in liquid nitrogen, crushing, and performing supercritical extraction to obtain tea leaf extract;
step two: mixing the tea extract with caprylic/capric glyceride according to a weight ratio of 1:5 to form an oil phase;
step three: adding the nanoparticle modified beta-cyclodextrin into 3 times of water to form a water phase;
step four: heating the oil phase prepared in the second step to 50 ℃, then adding the oil phase into the water phase prepared in the third step, shearing and homogenizing the oil phase, wherein the rotating speed of shearing and homogenizing is increased to 10000r/min, and shearing and homogenizing the oil phase for 25min to obtain a premix emulsion;
step five: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
The modification method of the nanoparticle modified beta-cyclodextrin comprises the following steps:
s101: peeling rhizoma Dioscoreae, pulping in 3 times of water, filtering to obtain filtrate, adding 5% sodium alginate, and stirring to obtain rhizoma Dioscoreae extractive solution;
s102: adding chitosan into acetic acid to prepare a chitosan solution with the mass fraction of 5%, and then mixing the chitosan solution and the yam extracting solution according to the weight ratio of 5:1 to obtain a modified solution;
s103: adding beta-cyclodextrin into 20% of nano tricalcium phosphate modifier, stirring and mixing thoroughly to obtain nano tricalcium phosphate composite beta-cyclodextrin;
s104: s103, mixing the product and the modifying liquid according to the weight ratio of 1:5, mixing, stirring and reacting for 20min at 60 ℃, after stirring, washing with water and drying to obtain the modified beta-cyclodextrin.
The preparation method of the nano tricalcium phosphate modifier in the embodiment comprises the following steps: 10 parts of nano tricalcium phosphate is sent into 15 parts of hydrochloric acid solution with the mass fraction of 2%, 1 part of CMC-Na and 1 part of sodium citrate are added, and the mixture is stirred and mixed fully, washed and dried to obtain the nano tricalcium phosphate modifier.
The particle size of the nano tricalcium phosphate of this example was 10nm.
The specific operation steps of the supercritical preparation technology of the embodiment are as follows:
injecting the premix into a carbon dioxide fluid reaction kettle at 300K and 9MPa under CO 2 Treating for 30min under the condition of flow velocity to obtain a suspension;
and (5) washing the suspension for multiple times by using distilled water, and freeze-drying to obtain microcapsule powder.
CO of the present embodiment 2 The flow rate was 0.4L/min.
The tea extract prepared by the preparation method of the microcapsule powder containing the tea extract is provided.
The microcapsule powder is applied to beverages, ice cream, cakes and dairy foods.
Example 2.
The invention provides a preparation method of microcapsule powder containing tea extract, which comprises the following steps:
step one: washing tea leaves with water, draining, freezing in liquid nitrogen, crushing, and performing supercritical extraction to obtain tea leaf extract;
step two: mixing the tea extract with caprylic/capric glyceride according to a weight ratio of 1:5 to form an oil phase;
step three: adding the nanoparticle modified beta-cyclodextrin into 6 times of water to form a water phase;
step four: heating the oil phase prepared in the second step to 70 ℃, then adding the oil phase into the water phase prepared in the third step, shearing, homogenizing at 20000r/min, shearing, homogenizing for 35min to obtain a premix;
step five: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
The modification method of the nanoparticle modified beta-cyclodextrin comprises the following steps:
s101: peeling rhizoma Dioscoreae, pulping in 3 times of water, filtering to obtain filtrate, adding 10% sodium alginate, and stirring to obtain rhizoma Dioscoreae extractive solution;
s102: adding chitosan into acetic acid to prepare a chitosan solution with the mass fraction of 5%, and then mixing the chitosan solution and the yam extracting solution according to the weight ratio of 5:1 to obtain a modified solution;
s103: adding beta-cyclodextrin into 30% of nano tricalcium phosphate modifier, stirring and mixing thoroughly to obtain nano tricalcium phosphate composite beta-cyclodextrin;
s104: s103, mixing the product and the modifying liquid according to the weight ratio of 1:7, mixing, stirring and reacting for 30min at 85 ℃, after stirring, washing with water and drying to obtain the modified beta-cyclodextrin.
The preparation method of the nano tricalcium phosphate modifier in the embodiment comprises the following steps: and (3) adding 20 parts of nano tricalcium phosphate into 25 parts of hydrochloric acid solution with the mass fraction of 2%, adding 5 parts of CMC-Na and 3 parts of sodium citrate, stirring and mixing fully, washing with water, and drying to obtain the nano tricalcium phosphate modifier.
The particle size of the nano tricalcium phosphate of this example was 30nm.
The specific operation steps of the supercritical preparation technology of the embodiment are as follows:
injecting the premix into a carbon dioxide fluid reaction kettle at 330K and 12MPa under CO 2 Treating for 60min under the condition of flow velocity to obtain a suspension;
and (5) washing the suspension for multiple times by using distilled water, and freeze-drying to obtain microcapsule powder.
CO of the present embodiment 2 The flow rate was 0.7L/min.
The tea extract prepared by the preparation method of the microcapsule powder containing the tea extract is provided.
The microcapsule powder is applied to beverages, ice cream, cakes and dairy foods.
Example 3.
The invention provides a preparation method of microcapsule powder containing tea extract, which comprises the following steps:
step one: washing tea leaves with water, draining, freezing in liquid nitrogen, crushing, and performing supercritical extraction to obtain tea leaf extract;
step two: mixing the tea extract with caprylic/capric glyceride according to a weight ratio of 1:5 to form an oil phase;
step three: adding the nanoparticle modified beta-cyclodextrin into 4.5 times of water to form a water phase;
step four: heating the oil phase prepared in the second step to 60 ℃, then adding the oil phase into the water phase prepared in the third step, shearing and homogenizing the oil phase, wherein the rotating speed of shearing and homogenizing is increased to 15000r/min, and shearing and homogenizing the oil phase for 30min to obtain a premix emulsion;
step five: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
The modification method of the nanoparticle modified beta-cyclodextrin comprises the following steps:
s101: peeling rhizoma Dioscoreae, pulping in 3 times of water, filtering to obtain filtrate, adding 7.5% sodium alginate, and stirring to obtain rhizoma Dioscoreae extractive solution;
s102: adding chitosan into acetic acid to prepare a chitosan solution with the mass fraction of 5%, and then mixing the chitosan solution and the yam extracting solution according to the weight ratio of 5:1 to obtain a modified solution;
s103: adding beta-cyclodextrin into 25% of nano tricalcium phosphate modifier, stirring and mixing thoroughly to obtain nano tricalcium phosphate composite beta-cyclodextrin;
s104: s103, mixing the product and the modifying liquid according to the weight ratio of 1:6, mixing, stirring and reacting for 25min at 75 ℃, after stirring, washing with water and drying to obtain the modified beta-cyclodextrin.
The preparation method of the nano tricalcium phosphate modifier in the embodiment comprises the following steps: 15 parts of nano tricalcium phosphate is sent into 20 parts of hydrochloric acid solution with the mass fraction of 2%, 3 parts of CMC-Na and 2 parts of sodium citrate are added, and the mixture is stirred and mixed fully, washed and dried to obtain the nano tricalcium phosphate modifier.
The particle size of the nano tricalcium phosphate of this example was 20nm.
The specific operation steps of the supercritical preparation technology of the embodiment are as follows:
injecting the premix into a carbon dioxide fluid reaction kettle at 315K and 10MPa under CO 2 Treating for 45min under the condition of flow velocity to obtain a suspension;
and (5) washing the suspension for multiple times by using distilled water, and freeze-drying to obtain microcapsule powder.
CO of the present embodiment 2 The flow rate was 0.55L/min.
The tea extract prepared by the preparation method of the microcapsule powder containing the tea extract is provided.
The microcapsule powder is applied to beverages, ice cream, cakes and dairy foods.
Example 4.
The invention provides a preparation method of microcapsule powder containing tea extract, which comprises the following steps:
step one: washing tea leaves with water, draining, freezing in liquid nitrogen, crushing, and performing supercritical extraction to obtain tea leaf extract;
step two: mixing the tea extract with caprylic/capric glyceride according to a weight ratio of 1:5 to form an oil phase;
step three: adding the nanoparticle modified beta-cyclodextrin into 5 times of water to form a water phase;
step four: heating the oil phase prepared in the second step to 65 ℃, then adding the oil phase into the water phase prepared in the third step, shearing and homogenizing the oil phase, wherein the rotating speed of shearing and homogenizing is increased to 17000r/min, and shearing and homogenizing the oil phase for 35min to obtain a premix emulsion;
step five: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
The modification method of the nanoparticle modified beta-cyclodextrin comprises the following steps:
s101: peeling rhizoma Dioscoreae, pulping in 3 times of water, filtering to obtain filtrate, adding 8% sodium alginate, and stirring to obtain rhizoma Dioscoreae extractive solution;
s102: adding chitosan into acetic acid to prepare a chitosan solution with the mass fraction of 5%, and then mixing the chitosan solution and the yam extracting solution according to the weight ratio of 5:1 to obtain a modified solution;
s103: adding beta-cyclodextrin into 22% of nano tricalcium phosphate modifier, stirring and mixing thoroughly to obtain nano tricalcium phosphate composite beta-cyclodextrin;
s104: s103, mixing the product and the modifying liquid according to the weight ratio of 1:5, mixing, stirring and reacting for 30min at 80 ℃, after stirring, washing with water, and drying to obtain the modified beta-cyclodextrin.
The preparation method of the nano tricalcium phosphate modifier in the embodiment comprises the following steps: and (3) conveying 12 parts of nano tricalcium phosphate into 18 parts of hydrochloric acid solution with the mass fraction of 2%, adding 2 parts of CMC-Na and 2 parts of sodium citrate, stirring and mixing fully, and then washing and drying to obtain the nano tricalcium phosphate modifier.
The particle size of the nano tricalcium phosphate of this example was 20nm.
The specific operation steps of the supercritical preparation technology of the embodiment are as follows:
injecting the premix into a carbon dioxide fluid reaction kettle at a temperature of 310K and a pressure of 9MPa and CO 2 Treating for 50min under the condition of flow velocity to obtain a suspension;
and (5) washing the suspension for multiple times by using distilled water, and freeze-drying to obtain microcapsule powder.
CO of the present embodiment 2 The flow rate was 0.5L/min.
The tea extract prepared by the preparation method of the microcapsule powder containing the tea extract is provided.
The microcapsule powder is applied to beverages, ice cream, cakes and dairy foods.
Example 5.
The invention provides a preparation method of microcapsule powder containing tea extract, which comprises the following steps:
step one: washing tea leaves with water, draining, freezing in liquid nitrogen, crushing, and performing supercritical extraction to obtain tea leaf extract;
step two: mixing the tea extract with caprylic/capric glyceride according to a weight ratio of 1:5 to form an oil phase;
step three: adding the nanoparticle modified beta-cyclodextrin into 4 times of water to form a water phase;
step four: heating the oil phase prepared in the second step to 55 ℃, then adding the oil phase into the water phase prepared in the third step, shearing and homogenizing the oil phase, wherein the rotating speed of shearing and homogenizing is increased to 19000r/min, and shearing and homogenizing the oil phase for 33min to obtain a premix emulsion;
step five: the pre-mixed emulsion is treated by adopting a supercritical preparation technology to obtain the microcapsule powder.
The modification method of the nanoparticle modified beta-cyclodextrin comprises the following steps:
s101: peeling rhizoma Dioscoreae, pulping in 3 times of water, filtering to obtain filtrate, adding 9% sodium alginate, and stirring to obtain rhizoma Dioscoreae extractive solution;
s102: adding chitosan into acetic acid to prepare a chitosan solution with the mass fraction of 5%, and then mixing the chitosan solution and the yam extracting solution according to the weight ratio of 5:1 to obtain a modified solution;
s103: adding the beta-cyclodextrin into 28% of nano tricalcium phosphate modifier, stirring and mixing fully to obtain nano tricalcium phosphate composite beta-cyclodextrin;
s104: s103, mixing the product and the modifying liquid according to the weight ratio of 1:6.5, mixing, stirring and reacting for 28min at 70 ℃, and after stirring, washing and drying to obtain the modified beta-cyclodextrin.
The preparation method of the nano tricalcium phosphate modifier in the embodiment comprises the following steps: and (3) feeding 18 parts of nano tricalcium phosphate into 22 parts of hydrochloric acid solution with the mass fraction of 2%, adding 4 parts of CMC-Na and 1 part of sodium citrate, stirring and mixing fully, washing with water, and drying to obtain the nano tricalcium phosphate modifier.
The particle size of the nano tricalcium phosphate of this example was 30nm.
The specific operation steps of the supercritical preparation technology of the embodiment are as follows:
injecting the premixed emulsion into a carbon dioxide fluid reaction kettle at 320K and 11MPa under CO 2 Treating for 40min under the condition of flow velocity to obtain suspension;
and (5) washing the suspension for multiple times by using distilled water, and freeze-drying to obtain microcapsule powder.
CO of the present embodiment 2 The flow rate was 0.6L/min.
The tea extract prepared by the preparation method of the microcapsule powder containing the tea extract is provided.
The microcapsule powder is applied to beverages, ice cream, cakes and dairy foods.
Comparative example 1.
The difference from example 4 is that the nanoparticle modified beta-cyclodextrin is replaced by beta-cyclodextrin.
Comparative example 2.
The difference from example 4 is that nano calcium carbonate powder is used instead of nano tricalcium phosphate in the modification of nano particle modified beta-cyclodextrin.
Comparative example 3.
The difference from example 4 is that the yam extract is not added in the modification of the nanoparticle modified beta-cyclodextrin.
Comparative example 4.
In the preparation of the nano tricalcium phosphate modifier, the nano tricalcium phosphate is adopted to be fully stirred and dispersed in a chitosan aqueous solution with the mass fraction of 10 percent which is 2-3 times that of the nano tricalcium phosphate, and then the nano tricalcium phosphate modifier is obtained after water washing and drying.
Comparative example 5.
Unlike example 4, no supercritical formulation technique was employed, but spray drying was employed.
The products of examples 1-5 and comparative examples 1-5 were subjected to a tea aroma dissolution performance test; taking the total content of nerolidol, phytol and farnesene as an example, the performance test is carried out:
the product properties of examples 1-5 and comparative examples 1-5 were tested as follows:
as can be seen from comparative example 1 and example 4, the nanoparticle modified beta-cyclodextrin is replaced by beta-cyclodextrin, the product has burst release phenomenon in 1 month, the release amount of the tea fragrance is faster and larger, and the stability performance is reduced;
meanwhile, the nano particle modified beta-cyclodextrin modification is not added with yam extracting solution, nano particles are replaced by nano calcium carbonate, and the stability of the product is reduced to different degrees;
and the nano tricalcium phosphate prepared by adopting other methods has remarkable improvement effect compared with the invention, and the stability is optimal by adopting the preparation method of the invention.
Compared with the common spray drying, the supercritical preparation technology has obvious effect, better stability and better protection of tea fragrance;
in addition, the dissolution rate of the product in the embodiment 4 of the invention can reach 9.8% after 6 months, the best stability is realized, the original flavor of tea can be retained to the greatest extent, and the dissolution rate is reduced to different degrees by adopting a comparative example scheme.
The flavor test results of examples 1-5 and comparative examples 1-5 are as follows
Water is mixed with: erythritol: product = 80:16:4 formulated beverage for testing:
consumer preference test
Randomly selecting 200 consumption groups, wherein 100 consumption groups are respectively selected, the ages of men and women are respectively half, the ages are 15-65 years, and the beverage products are respectively used as test objects to test the preference degree of each group of beverage;
like: the taste and the flavor of the beverage are accepted, and the beverage is willing to be consumed;
generally: the taste and the flavor of the beverage are compared and accepted;
dislike: the taste and the flavor of the beverage are not accepted, and the beverage is not willing to consume;
the beverage of the product has a favorite number of 86 people, and the beverage of the market has a favorite number of 73 people and a dislike number of 8 people, so that the beverage of the invention has great advantage in competition in the market.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (5)
1. The preparation method of the microcapsule powder containing the tea extract is characterized by comprising the following steps of:
step one: washing tea leaves with water, draining, freezing in liquid nitrogen, crushing, and performing supercritical extraction to obtain tea leaf extract;
step two: mixing the tea extract with caprylic/capric glyceride according to a weight ratio of 1:5 to form an oil phase;
step three: adding the nanoparticle modified beta-cyclodextrin into 3-6 times of water to form a water phase;
step four: heating the oil phase prepared in the second step to 50-70 ℃, then adding the oil phase into the water phase prepared in the third step, shearing and homogenizing the oil phase to 10000-20000r/min, shearing and homogenizing the oil phase for 25-35min to obtain a premix emulsion;
step five: treating the premix by adopting a supercritical preparation technology to obtain microcapsule powder; the modification method of the nanoparticle modified beta-cyclodextrin comprises the following steps:
s101: peeling rhizoma Dioscoreae, pulping in 3 times of water, filtering to obtain filtrate, adding 5-10% sodium alginate, and stirring to obtain rhizoma Dioscoreae extractive solution;
s102: adding chitosan into acetic acid to prepare a chitosan solution with the mass fraction of 5%, and then mixing the chitosan solution and the yam extracting solution according to the weight ratio of 5:1 to obtain a modified solution;
s103: adding beta-cyclodextrin into 20-30% of nano tricalcium phosphate modifier, stirring and mixing thoroughly to obtain nano tricalcium phosphate composite beta-cyclodextrin;
s104: s103, mixing the product and the modifying liquid according to the weight ratio of 1: (5-7) mixing, stirring at 60-85 ℃ for reaction for 20-30min, washing with water and drying to obtain modified beta-cyclodextrin; the preparation method of the nano tricalcium phosphate improver comprises the following steps: 10-20 parts of nano tricalcium phosphate is sent into 15-25 parts of hydrochloric acid solution with the mass fraction of 2%, 1-5 parts of CMC-Na and 1-3 parts of sodium citrate are added, stirred and mixed fully, and then washed and dried to obtain the nano tricalcium phosphate modifier; the supercritical preparation technology comprises the following specific operation steps:
injecting the premixed emulsion into a carbon dioxide fluid reaction kettle at 300-330K and 9-12MPa under CO 2 Treating for 30-60min under the condition of flow velocity to obtain suspension;
and (5) washing the suspension for multiple times by using distilled water, and freeze-drying to obtain microcapsule powder.
2. The method for preparing microcapsule powder containing tea extract according to claim 1, wherein the particle size of the nano tricalcium phosphate is 10-30nm.
3. A process for the preparation of a microcapsule powder comprising tea leaf extract as claimed in claim 1, wherein the CO 2 The flow rate is 0.4-0.7L/min.
4. A tea extract-containing microcapsule powder prepared by the method for preparing a tea extract-containing microcapsule powder as claimed in any one of claims 1-3.
5. Use of the microcapsule powder according to claim 4 for preparing beverages, cakes, dairy foods.
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| KR20030025606A (en) * | 2001-09-21 | 2003-03-29 | 한미향료화학주식회사 | Method of refining and microcapsuling tea extract |
| CN109757590A (en) * | 2019-03-19 | 2019-05-17 | 浙江亚林生物科技股份有限公司 | A kind of preparation method of natural tea essence |
| CN112167598A (en) * | 2020-10-15 | 2021-01-05 | 吉源(淮北)食品科技有限公司 | Preparation method of microcapsule particle slow-release coating essence |
| CN112536005A (en) * | 2020-11-05 | 2021-03-23 | 华南理工大学 | Starch-embedded fragrant substance microcapsule and preparation method thereof |
| CN114958482A (en) * | 2022-06-29 | 2022-08-30 | 湖南金宝来香业有限公司 | Preparation method of perfume with lasting fragrance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20030025606A (en) * | 2001-09-21 | 2003-03-29 | 한미향료화학주식회사 | Method of refining and microcapsuling tea extract |
| CN109757590A (en) * | 2019-03-19 | 2019-05-17 | 浙江亚林生物科技股份有限公司 | A kind of preparation method of natural tea essence |
| CN112167598A (en) * | 2020-10-15 | 2021-01-05 | 吉源(淮北)食品科技有限公司 | Preparation method of microcapsule particle slow-release coating essence |
| CN112536005A (en) * | 2020-11-05 | 2021-03-23 | 华南理工大学 | Starch-embedded fragrant substance microcapsule and preparation method thereof |
| CN114958482A (en) * | 2022-06-29 | 2022-08-30 | 湖南金宝来香业有限公司 | Preparation method of perfume with lasting fragrance |
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