CN109452427A - Health care emperor chrysanthemum tea and its preparation process - Google Patents
Health care emperor chrysanthemum tea and its preparation process Download PDFInfo
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Abstract
The invention discloses a kind of health care emperor chrysanthemum tea and its preparation processes.The preparation process of the health care emperor chrysanthemum tea, comprising the following steps: pick, spread, flower, just baking, multiple baking, final firing only.Health care emperor chrysanthemum tea petal of the present invention is completely without crimping, without obvious drying shrinkage, rear flower golden yellow color is brewed, soup look is limpid bright, and fragrance faint scent is lasting, flavour glycol, there is antibacterial, eliminate free radical, anti-oxidant and antineoplastic action containing nutritional ingredients such as flavonoids, terpene, amino acids and green onion quinones chemicals with the distinctive astringent taste of chrysanthemum, it can be relieved stress with pleasure mood.
Description
Technical field
The present invention relates to tea-drinking technical fields, more particularly to a kind of health care emperor chrysanthemum tea and its preparation process.
Background technique
Chrysanthemum is composite family herbaceos perennial, is traditional one of the parts of generic medicinal plants in China, is mainly supplied with capitulum
It is medicinal.Recorded according to ancient books, chrysanthemum sweet-bitter flavor, cold nature, have relieve heat heat-clearing, clear liver and improve vision and the effects of detoxicating, relieving inflammation, to dry,
Hyperactivity of fire, mesh are puckery, or have certain curative effect by chill, wet caused limbs pain, numb disease.Cure mainly cold anemopyretic, head
Slight illness etc. has preventive and therapeutic effect to dizziness, headache, tinnitus.
Chrysanthemum is divided into mother chrysanthemum and family chrysanthemum, and family chrysanthemum clears liver and improve vision, and mother chrysanthemum toxic removing dissipates fire, and sweetness and bitterness is slightly cold, clearing heat and detoxicating, to eye
Mirror strain, headache, hypertension etc. have certain effectiveness.The drug effect of chrysanthemum tea is also documented in detail in Compendium of Material Medica: property
Glycosides, it is slightly cold, there is the effect of dissipating wind-heat, calming the liver and improving eyesight.Shennong's Herbal thinks, feverfew jasmine tea can " Chu's wind headache, swelling and pain,
Mesh is intended to take off, the dead flesh of skin, foul wind arthritis with fixed pain caused by dampness, long term usage benefit gas, macrobiosis of enduring hardships of making light of one's life by commiting suicide."
In chrysanthemum containing volatile oil, chrysanthemum glycosides, adenine, amino acid, choline, stachydrine, flavonoids, asterin, vitamin,
The substances such as microelement, can antipathogen, enhance capillary resistance；Flavonoid substances therein are it is verified that freedom
Base has a very strong scavenging effect, and it is anti-oxidant, in terms of it is fruitful.From nutrition angle analysis, plant
Essence is flowers and fruits.Contain amino acid in 17 in Chrysanthemum Petal, Glutamic Acid, aspartic acid, proline equal size are higher.This
Outside, vitamin and iron, zinc, copper, selenium and other trace elements are also rich in, thus have the function of that general vegetables are incomparable.
Summary of the invention
As the improvement of people's living standards, being no longer limited only to medicinal health function to drinking for chrysanthemum tea now.Institute
Other than requiring chrysanthemum tea that there is consumption value, it is also necessary to which it has preferable ornamental value.
The first object of the present invention is to provide a kind of preparation process of health care emperor chrysanthemum tea, by absorbing the excellent of traditional handicraft
Gesture overcomes deficiency, obtains with health care emperor's chrysanthemum tea at shape.
The processing technology of traditional chrysanthemum tea generally pick flowers → steam and spend → dry → receive flower, the chrysanthemum tea of production has the fragrance of a flower,
Leaf color is uniform, and soup look Huang is bright, but lacks ornamental value after brewing.
The invention discloses a kind of preparation processes of health care emperor chrysanthemum tea, comprising the following steps: picks, spreads, spending only, just
It dries, multiple baking, final firing.
Specifically, the preparation process of the health care emperor chrysanthemum tea, comprising the following steps:
Step S1 picking: emperor's daisy_petal part unfold it is straight, fickle in love scatter 80~90% when, both hands are held flower and are picked；
Step S2 is spread: upward by emperor's radial striations, being spread 10~15 hours at 20~35 DEG C of temperature；
Step S3 is spent only: being cleared up the impurity of emperor chrysanthemum surface attachment, is then uniformly placed on stoving rack；
Step S4 just dries: just dry with dryer, 40~45 DEG C of temperature, is dried to water content and reaches 40~50%, with
Timely airing afterwards, 20~35 DEG C of airing temperature, the airing time 60~90 minutes；
Step S5 dries again: multiple baking carried out with dryer, 45~50 DEG C of temperature, water content is dried to and reaches 15~20%, with
Timely airing afterwards, 20~35 DEG C of airing temperature, the airing time 60~90 minutes；
Step S6 final firing: final firing is carried out with dryer, 60~65 DEG C of temperature, water content is dried to and reaches 9~10%, then
Timely airing, the airing time 80~100 minutes, obtains the health care emperor chrysanthemum tea by 20~35 DEG C of airing temperature.
The above method is omitted high temperature and steams flower process, first by spreading, extends process time, promotes chrysanthemum internal component
Conversion；Then baking process is stepped up using segmentation drying by temperature, is conducive to scattering and disappearing and aroma substance for moisture
Aggregation；Then higher temperature final firing is used, so that low melting point aromatic substance comparatively fast volatilizees, the fragrance of a flower is more pure and mild, brews rear fragrance
It volatilizees more prominent.The chrysanthemum tea obtained using this method, which is had, is completely suitable for consumer at a shape, fragrance and flavour
Group.
Further, the preparation process of the health care emperor chrysanthemum tea, comprising the following steps:
Step S1 picking: emperor's daisy_petal part unfold it is straight, fickle in love scatter 80~90% when, both hands are held flower and are picked；
Step S2 is spread: upward by emperor's radial striations, being spread 10~15 hours at 20~35 DEG C of temperature；
Step S3 is spent only: being cleared up the impurity of emperor chrysanthemum surface attachment, is then uniformly placed on stoving rack；
The protection of step S4 nutritional ingredient: emperor chrysanthemum is impregnated 5~10 minutes in nutritional ingredient protection liquid, takes out, drains；
Step S5 just dries: just dry with dryer, 40~45 DEG C of temperature, is dried to water content and reaches 40~50%, with
Timely airing afterwards, 20~35 DEG C of airing temperature, the airing time 60~90 minutes；
Step S6 dries again: multiple baking carried out with dryer, 45~50 DEG C of temperature, water content is dried to and reaches 15~20%, with
Timely airing afterwards, 20~35 DEG C of airing temperature, the airing time 60~90 minutes；
Step S7 final firing: final firing is carried out with dryer, 60~65 DEG C of temperature, water content is dried to and reaches 9~10%, then
Timely airing, the airing time 80~100 minutes, obtains the health care emperor chrysanthemum tea by 20~35 DEG C of airing temperature.
As one of currently preferred technical solution, the preparation process of the nutritional ingredient protection liquid are as follows: weigh grape
0.2~0.3g of saccharic acid lactone, 0.4~0.45g of niacinamide, 20~50 μ L of phytic acid, 3~5g of immobilised enzymes, 1~2g of chitosan are mixed
After conjunction, water is added to be settled to 100mL.
By the present invention in that being obtained with specific compositions such as glucolactone, immobilised enzymes, niacinamide, phytic acid and chitosans
Nutritional ingredient protect liquid, play good antioxidation.In the preparation process of health care emperor chrysanthemum tea of the present invention, not only avoid
Steaming step using high temperature prevents from destroying chrysanthemum effective component, and protects liquid processing by nutritional ingredient, prevents in chrysanthemum
Active constituent especially Flavonoid substances are oxidized destruction, play a very good protection.Wherein glucolactone and plant
Acid has faintly acid, so it is not high using content.
As one of currently preferred technical solution, the preparation process of the nutritional ingredient protection liquid are as follows: weigh grape
0.2~0.3g of saccharic acid lactone, 0.4~0.45g of niacinamide, 20~50 μ L of phytic acid, 3~5g of immobilised enzymes, chitosan 0.3~
0.6g, 1~3 μ L of aromatic alkyl glucoside, after mixing, add water to be settled to 100mL.
Aromatic alkyl glucoside not only has flavouring effect, but also can play bacteriostasis, while preventing lipophilicity
Active material destroyed, volatility resistance effect more makes it with inoxidizability.By aromatic alkyl Portugal in the present invention
Polyglycoside is applied in the preparation process of chrysanthemum tea, plays the role of flavouring, anti-corrosion, anti-oxidant three unification, effective protection
Chrysanthemum active constituent is destroyed, where this is one of innovation of the invention.
As one of currently preferred technical solution, the preparation process of the nutritional ingredient protection liquid are as follows: weigh grape
0.2~0.3g of saccharic acid lactone, 0.4~0.45g of niacinamide, 20~50 μ L of phytic acid, 3~5g of immobilised enzymes, folacin coupled chitosan
0.3~0.6g, 1~3 μ L of aromatic alkyl glucoside, after mixing, add water to be settled to 100mL.
The aromatic alkyl glucoside is benzyl alcohol-beta-glucosidase and/or benzyl carbinol-β-D glucoside.It is preferred that
Ground, the aromatic alkyl glucoside are that benzyl alcohol-beta-glucosidase and benzyl carbinol-β-D glucoside are formed with volume ratio 1:1
Mixture.
The folacin coupled chitosan is prepared by the following method: weighing 2.6~2.8g folic acid and 2.6~2.8g 1- (3-
Dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride, it is dissolved in 100~150mL anhydrous dimethyl sulphoxide, in light protected environment
It is stirred 40~60 minutes in 20~30 DEG C, obtains folic acid solution；2.6~2.8g chitosan is weighed, pH4.7, molar concentration are dissolved in
0.2mol/L NaAc_HAc buffer solution stirs 10~20 minutes, and the chitosan for obtaining mass fraction 0.3~0.5% is molten
Liquid；Folic acid solution is added in chitosan solution, is stirred to react 12~16 hours；To after reaction, adjust the pH of reaction solution
To 8~9, then successively dialysed 3~4 days with the phosphate buffer of pH7.4, distilled water, it is even to obtain the folic acid for freeze-drying
Join chitosan.Nitrogen-atoms on folic acid and chitosan reacts, and obtains folacin coupled chitosan, is used in chrysanthemum tea
When in preparation, the soup look of chrysanthemum leaching liquor be improved significantly, thus it is speculated that its reason is whether may be the oxidation of Flavonoid substances
An important factor for influencing soup look, and folacin coupled chitosan imparts its faintly acid, is more advantageous to nutritional ingredient protection liquid antioxygen
Change the performance of effect.
In the above technical solution, the immobilised enzymes can both select immobilized tannase, immobilization glycosidase, consolidate
Surely change one of anthocyanin reductase, it can also be using the immobilization complex enzyme used in the present invention.
The preparation process of the immobilization complex enzyme are as follows: tannase plus water are configured to the tannin enzyme solution of 0.1mg/mL；It will
Anthocyanin reductase adds water to be configured to the anthocyanin reductase liquid of 0.1mg/mL；By tannin enzyme solution 2.5mL, anthocyanin reductase liquid
2.5mL mixing, is added the sodium alginate aqueous solution 7mL of mass fraction 3%, mixes well；Mass fraction 2.5% is then added
Glutaraldehyde fixer makes the concentration of glutaraldehyde in the solution reach 1.25wt%；After being vibrated 30 minutes with 180 revs/min, in 20
DEG C stand crosslinking 4 hours, collect reaction solution；Reaction solution is used to the calcium chloride water of No. 5 syringe needle implantation quality scores 2%
In, it is centrifuged 15 minutes with 3000 revs/min, takes bottom solid；By bottom solid with the calcium chloride solution of mass fraction 2% 2
DEG C impregnate 2 hours, with 3000 revs/min be centrifuged 15 minutes, take bottom precipitation；By bottom precipitation mass fraction 0.075%
Glutaraldehyde solution is crosslinked 3 hours at 10 DEG C, is crossed 300 mesh filter screens, is taken filter cake；Filter cake is washed with the phosphate buffer of pH7.4
Afterwards, it drains away the water, obtains the immobilization complex enzyme.
The anthocyanin reductase is phenylalanine deaminase, cinnamic acid carboxylase, 4- coumaric acyl CoA ligase, looks into ear
Ketone synzyme, chalcone isomerase, flavanone 3- hydroxylase, flavanones 3 '-hydroxylase, 3 ', 5 '-hydroxylase of flavanones, two
One or more of hydrogen flavanols 4- reductase, leucoanthocyanidin reductase.
The immobilization complex enzyme for using tannase and anthocyanin reductase to obtain in the present invention as proenzyme material, chrysanthemum tea leaching
The quality of extract is significantly improved, and is on the one hand since immobilization complex enzyme can occur with the flocculation sedimentation in leaching liquor
Reaction generates the small water-soluble substances of relative molecular weight, achievees the purpose that clarify leaching liquor；It on the other hand is because immobilization is multiple
Synthase makes chrysanthemum internal substance obtain certain balance between hydrolysis and preservation, has not only assigned its fragrance, but also remain nutrition
Substance.
The second technical problem to be solved by the present invention is to provide a kind of health care emperor chrysanthemum tea, using any of the above-described kind of health care emperor
The preparation process of chrysanthemum tea processes to obtain.
Health care emperor chrysanthemum tea petal of the present invention completely brews rear flower golden yellow color, soup look without obvious drying shrinkage without crimping
Limpid bright, fragrance faint scent is lasting, flavour glycol, have the distinctive astringent taste of chrysanthemum, containing flavonoids, terpene, amino acids and
The nutritional ingredients such as green onion quinones chemicals have antibacterial, eliminate free radical, anti-oxidant and antineoplastic action, can be with the pleasant heart
Feelings relieve stress.
Specific embodiment
Raw material is described below in embodiment:
Emperor chrysanthemum, the specific selenium-rich florists Chrysould likehemum using Tree in Enshi of Hubei Province plantation.
Glucolactone (i.e. gluconic acid-α-lactone), No. CAS: 90-80-2, food-grade.
Niacinamide, No. CAS: 98-92-0, food-grade.
Phytic acid, No. CAS: 83-86-3, food-grade.
Chitosan, No. CAS: 9012-76-4, food-grade.
Anhydrous sodium acetate, No. CAS: 127-09-3.
DEXTROSE ANHYDROUS, No. CAS: 50-99-7.
Benzyl alcohol, No. CAS: 100-51-6.
Boron trifluoride ether, No. CAS: 109-63-7.
Folic acid, No. CAS: 59-30-3, food-grade.
1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride, No. CAS: 25952-53-8.
PH4.7, molar concentration 0.2mol/L NaAc_HAc buffer solution are 0.2mol/L by 10.9mL molar concentration
Sodium acetate solution and 9.1mL molar concentration be 0.2mol/L acetum be uniformly mixed obtain.
The phosphate buffer of pH7.4 is rubbed by disodium phosphate soln and 20mL that 80mL molar concentration is 0.2mol/L
The potassium dihydrogen phosphate that your concentration is 0.2mol/L, which is uniformly mixed, to be obtained.
2 phenylethyl alcohol, No. CAS: 60-12-8.
Tannase is specifically provided by Henan Hua Chi Biotechnology Co., Ltd, 800,000/g of enzyme activity.
Anthocyanin reductase specifically uses phenylalanine deaminase, is provided by Shanghai Bang Jing Industrial Co., Ltd., enzyme activity
600000/g.
In the case where not illustrating, the concrete technology condition of freeze-drying are as follows: -80 DEG C of pre-freezing temperature, when pre-freeze
Between 2 hours, -70 DEG C of cryogenic temperature, cooling time 48 hours, absolute pressure 100Pa.
Embodiment 1
The preparation process of health care emperor's chrysanthemum tea, comprising the following steps:
Step S1 picking: emperor's daisy_petal part unfold it is straight, fickle in love scatter 90% when, both hands are held flower and are picked；
Step S2 is spread: upward by emperor's radial striations, being spread 10 hours at 30 DEG C of temperature；
Step S3 is spent only: being cleared up with the impurity that dust catcher adheres to emperor chrysanthemum surface, is then uniformly placed in stoving rack
On；
Step S4 just dries: just dry with dryer, 40 DEG C of temperature, is dried to water content and reaches 50%, subsequent booth in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S5 dries again: carrying out multiple baking with dryer, temperature 50 C is dried to water content and reaches 20%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S6 final firing: carrying out final firing with dryer, and temperature 60 C is dried to water content and reaches 10%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes, obtains the health care emperor chrysanthemum tea.
Embodiment 2
The preparation process of health care emperor's chrysanthemum tea, comprising the following steps:
Step S1 picking: emperor's daisy_petal part unfold it is straight, fickle in love scatter 90% when, both hands are held flower and are picked；
Step S2 is spread: upward by emperor's radial striations, being spread 10 hours at 30 DEG C of temperature；
Step S3 is spent only: being cleared up with the impurity that dust catcher adheres to emperor chrysanthemum surface, is then uniformly placed in stoving rack
On；
The protection of step S4 nutritional ingredient: emperor chrysanthemum is impregnated 5 minutes in nutritional ingredient protection liquid, and dipping temperature is 30 DEG C,
The solid-liquid ratio of emperor chrysanthemum and nutritional ingredient protection liquid is 1:10 (g/mL), takes out, drains；
Step S5 just dries: just dry with dryer, 40 DEG C of temperature, is dried to water content and reaches 50%, subsequent booth in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S6 dries again: carrying out multiple baking with dryer, temperature 50 C is dried to water content and reaches 20%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S7 final firing: carrying out final firing with dryer, and temperature 60 C is dried to water content and reaches 10%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes, obtains the health care emperor chrysanthemum tea.
The preparation process of the nutritional ingredient protection liquid are as follows: weigh glucolactone 0.2g, niacinamide 0.45g, phytic acid
30 μ L, immobilized tannase 3g, chitosan 0.6g, after mixing, add water to be settled to 100mL.
The preparation process of immobilized tannase are as follows: tannase plus water are configured to the tannin enzyme solution of 0.1mg/mL；By tannin
Enzyme solution 5mL mixing, is added the sodium alginate aqueous solution 7mL of mass fraction 3%, mixes well；Mass fraction 2.5% is then added
Glutaraldehyde fixer so that the concentration of glutaraldehyde in the solution is reached 1.25wt%；After being vibrated 30 minutes with 180 revs/min, in
20 DEG C of standings are crosslinked 4 hours, collect reaction solution；Reaction solution is used to the calcium chloride water of No. 5 syringe needle implantation quality scores 2%
In, it is centrifuged 15 minutes with 3000 revs/min, takes bottom solid；By bottom solid with the calcium chloride solution of mass fraction 2% 2
DEG C impregnate 2 hours, with 3000 revs/min be centrifuged 15 minutes, take bottom precipitation；By bottom precipitation mass fraction 0.075%
Glutaraldehyde solution is crosslinked 3 hours at 10 DEG C, is crossed 300 mesh filter screens, is taken filter cake；Filter cake is washed with the phosphate buffer of pH7.4
Afterwards, it drains away the water, obtains the immobilized tannase.
Embodiment 3
The preparation process of health care emperor's chrysanthemum tea, comprising the following steps:
Step S1 picking: emperor's daisy_petal part unfold it is straight, fickle in love scatter 90% when, both hands are held flower and are picked；
Step S2 is spread: upward by emperor's radial striations, being spread 10 hours at 30 DEG C of temperature；
Step S3 is spent only: being cleared up with the impurity that dust catcher adheres to emperor chrysanthemum surface, is then uniformly placed in stoving rack
On；
The protection of step S4 nutritional ingredient: emperor chrysanthemum is impregnated 5 minutes in nutritional ingredient protection liquid, and dipping temperature is 30 DEG C,
The solid-liquid ratio of emperor chrysanthemum and nutritional ingredient protection liquid is 1:10 (g/mL), takes out, drains；
Step S5 just dries: just dry with dryer, 40 DEG C of temperature, is dried to water content and reaches 50%, subsequent booth in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S6 dries again: carrying out multiple baking with dryer, temperature 50 C is dried to water content and reaches 20%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S7 final firing: carrying out final firing with dryer, and temperature 60 C is dried to water content and reaches 10%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes, obtains the health care emperor chrysanthemum tea.
The preparation process of the nutritional ingredient protection liquid are as follows: weigh glucolactone 0.2g, niacinamide 0.45g, phytic acid
30 μ L, immobilized tannase 3g, chitosan 0.6g, 2 μ L of benzyl alcohol-beta-glucosidase, after mixing, add water to be settled to 100mL.
The preparation process of immobilized tannase are as follows: tannase plus water are configured to the tannin enzyme solution of 0.1mg/mL；By tannin
Enzyme solution 5mL mixing, is added the sodium alginate aqueous solution 7mL of mass fraction 3%, mixes well；Mass fraction 2.5% is then added
Glutaraldehyde fixer so that the concentration of glutaraldehyde in the solution is reached 1.25wt%；After being vibrated 30 minutes with 180 revs/min, in
20 DEG C of standings are crosslinked 4 hours, collect reaction solution；Reaction solution is used to the calcium chloride water of No. 5 syringe needle implantation quality scores 2%
In, it is centrifuged 15 minutes with 3000 revs/min, takes bottom solid；By bottom solid with the calcium chloride solution of mass fraction 2% 2
DEG C impregnate 2 hours, with 3000 revs/min be centrifuged 15 minutes, take bottom precipitation；By bottom precipitation mass fraction 0.075%
Glutaraldehyde solution is crosslinked 3 hours at 10 DEG C, is crossed 300 mesh filter screens, is taken filter cake；Filter cake is washed with the phosphate buffer of pH7.4
Afterwards, it drains away the water, obtains the immobilized tannase.
Benzyl alcohol-beta-glucosidase obtains by the following method:
(1) 20g anhydrous sodium acetate and 25g DEXTROSE ANHYDROUS are mixed, is added in 125mL acetic anhydride, in stirring condition
Under be heated to reflux 3 hours；Then stop heating, obtained solution is poured into 1000mL ice water, stir 3 hours, there is crystal analysis
Out；Supernatant liquid is poured out, is rinsed and is crystallized with ice water, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, obtains crude product；It will be thick
Product tie product again in ethanol, in 60 DEG C, absolute pressure 0.07MPa drying 5 hours, obtain pentaacetylglucose；
(2) 4.5g pentaacetylglucose and 1.24g benzyl alcohol are added in 23mL anhydrous methylene chloride, mixing is equal
It is even；0.027g boron trifluoride ether is added, after 25 DEG C are stirred to react 24 hours, collects reaction solution；Reaction solution is successively used
The sodium bicarbonate aqueous solution of 50mL mass fraction 5% is extracted twice, and is merged organic phase, is obtained extract liquor；By its etc. of extract liquor
After the saturated saline solution washing of volume, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, light yellow oil is obtained；It will
Light yellow oil silica gel column chromatography separating purification, eluent are V (chloroform): V (methanol)=15:1, then acetone recrystallization,
In 60 DEG C, absolute pressure 0.07MPa drying 4 hours, tetra-acetylated-β-benzyl alcohol glucoside is obtained；
(3) tetra-acetylated benzyl alcohol glucoside is added in triethylamine solution, obtains molar concentration 4.5mmol/L's
Solution, the triethylamine solution is by methanol: triethylamine: water is mixed to get with volume ratio 8:1:1, and it is small to be stirred to react 24 in 20 DEG C
When；After reaction, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, crude product is obtained；Crude product silica gel column chromatography is separated pure
Change, eluent is V (chloroform): V (methanol)=12:1, then acetone ties product again, in 60 DEG C, absolute pressure 0.07MPa dry 4 it is small
When, obtain benzyl alcohol-beta-glucosidase.
Embodiment 4
The preparation process of health care emperor's chrysanthemum tea, comprising the following steps:
Step S1 picking: emperor's daisy_petal part unfold it is straight, fickle in love scatter 90% when, both hands are held flower and are picked；
Step S2 is spread: upward by emperor's radial striations, being spread 10 hours at 30 DEG C of temperature；
Step S3 is spent only: being cleared up with the impurity that dust catcher adheres to emperor chrysanthemum surface, is then uniformly placed in stoving rack
On；
The protection of step S4 nutritional ingredient: emperor chrysanthemum is impregnated 5 minutes in nutritional ingredient protection liquid, and dipping temperature is 30 DEG C,
The solid-liquid ratio of emperor chrysanthemum and nutritional ingredient protection liquid is 1:10 (g/mL), takes out, drains；
Step S5 just dries: just dry with dryer, 40 DEG C of temperature, is dried to water content and reaches 50%, subsequent booth in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S6 dries again: carrying out multiple baking with dryer, temperature 50 C is dried to water content and reaches 20%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S7 final firing: carrying out final firing with dryer, and temperature 60 C is dried to water content and reaches 10%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes, obtains the health care emperor chrysanthemum tea.
The preparation process of the nutritional ingredient protection liquid are as follows: weigh glucolactone 0.2g, niacinamide 0.45g, phytic acid
30 μ L, immobilized tannase 3g, folacin coupled chitosan 0.6g, 2 μ L of benzyl alcohol-beta-glucosidase, after mixing, add water to be settled to
100mL。
The preparation process of immobilized tannase are as follows: tannase plus water are configured to the tannin enzyme solution of 0.1mg/mL；By tannin
Enzyme solution 5mL mixing, is added the sodium alginate aqueous solution 7mL of mass fraction 3%, mixes well；Mass fraction 2.5% is then added
Glutaraldehyde fixer so that the concentration of glutaraldehyde in the solution is reached 1.25wt%；After being vibrated 30 minutes with 180 revs/min, in
20 DEG C of standings are crosslinked 4 hours, collect reaction solution；Reaction solution is used to the calcium chloride water of No. 5 syringe needle implantation quality scores 2%
In, it is centrifuged 15 minutes with 3000 revs/min, takes bottom solid；By bottom solid with the calcium chloride solution of mass fraction 2% 2
DEG C impregnate 2 hours, with 3000 revs/min be centrifuged 15 minutes, take bottom precipitation；By bottom precipitation mass fraction 0.075%
Glutaraldehyde solution is crosslinked 3 hours at 10 DEG C, is crossed 300 mesh filter screens, is taken filter cake；Filter cake is washed with the phosphate buffer of pH7.4
Afterwards, it drains away the water, obtains the immobilized tannase.
Benzyl alcohol-beta-glucosidase obtains by the following method:
(1) 20g anhydrous sodium acetate and 25g DEXTROSE ANHYDROUS are mixed, is added in 125mL acetic anhydride, in stirring condition
Under be heated to reflux 3 hours；Then stop heating, obtained solution is poured into 1000mL ice water, stir 3 hours, there is crystal analysis
Out；Supernatant liquid is poured out, is rinsed and is crystallized with ice water, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, obtains crude product；It will be thick
Product tie product again in ethanol, in 60 DEG C, absolute pressure 0.07MPa drying 5 hours, obtain pentaacetylglucose；
(2) 4.5g pentaacetylglucose and 1.24g benzyl alcohol are added in 23mL anhydrous methylene chloride, mixing is equal
It is even；0.027g boron trifluoride ether is added, after 25 DEG C are stirred to react 24 hours, collects reaction solution；Reaction solution is successively used
The sodium bicarbonate aqueous solution of 50mL mass fraction 5% is extracted twice, and is merged organic phase, is obtained extract liquor；By its etc. of extract liquor
After the saturated saline solution washing of volume, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, light yellow oil is obtained；It will
Light yellow oil silica gel column chromatography separating purification, eluent are V (chloroform): V (methanol)=15:1, then acetone recrystallization,
In 60 DEG C, absolute pressure 0.07MPa drying 4 hours, tetra-acetylated-β-benzyl alcohol glucoside is obtained；
(3) tetra-acetylated benzyl alcohol glucoside is added in triethylamine solution, obtains molar concentration 4.5mmol/L's
Solution, the triethylamine solution is by methanol: triethylamine: water is mixed to get with volume ratio 8:1:1, and it is small to be stirred to react 24 in 20 DEG C
When；After reaction, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, crude product is obtained；Crude product silica gel column chromatography is separated pure
Change, eluent is V (chloroform): V (methanol)=12:1, then acetone ties product again, in 60 DEG C, absolute pressure 0.07MPa dry 4 it is small
When, obtain benzyl alcohol-beta-glucosidase.
Folacin coupled chitosan is prepared by the following method: weighing 2.6g folic acid and 2.7g 1- (3- dimethylamino-propyl)-
3- ethyl-carbodiimide hydrochloride is dissolved in 100mL anhydrous dimethyl sulphoxide, is stirred in light protected environment in 25 DEG C with 100 revs/min
It mixes 40 minutes, obtains folic acid solution；2.6g chitosan is weighed, it is slow to be dissolved in pH4.7, molar concentration 0.2mol/L Acetic acid-sodium acetate
Solution is rushed, is stirred 20 minutes with 100 revs/min, obtains the chitosan solution of mass fraction 0.5%；Shell is added in folic acid solution
In glycan solution, it is stirred to react 16 hours with 100 revs/min；To after reaction, use the hydroxide of molar concentration 1mol/L
Sodium water solution adjusts the pH to 9 of reaction solution, is then successively dialysed 3 days with the phosphate buffer of pH7.4, distilled water, freezing is dry
It is dry, obtain the folacin coupled chitosan.
Embodiment 5
The preparation process of health care emperor's chrysanthemum tea, comprising the following steps:
Step S1 picking: emperor's daisy_petal part unfold it is straight, fickle in love scatter 90% when, both hands are held flower and are picked；
Step S2 is spread: upward by emperor's radial striations, being spread 10 hours at 30 DEG C of temperature；
Step S3 is spent only: being cleared up with the impurity that dust catcher adheres to emperor chrysanthemum surface, is then uniformly placed in stoving rack
On；
The protection of step S4 nutritional ingredient: emperor chrysanthemum is impregnated 5 minutes in nutritional ingredient protection liquid, and dipping temperature is 30 DEG C,
The solid-liquid ratio of emperor chrysanthemum and nutritional ingredient protection liquid is 1:10 (g/mL), takes out, drains；
Step S5 just dries: just dry with dryer, 40 DEG C of temperature, is dried to water content and reaches 50%, subsequent booth in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S6 dries again: carrying out multiple baking with dryer, temperature 50 C is dried to water content and reaches 20%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S7 final firing: carrying out final firing with dryer, and temperature 60 C is dried to water content and reaches 10%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes, obtains the health care emperor chrysanthemum tea.
The preparation process of the nutritional ingredient protection liquid are as follows: weigh glucolactone 0.2g, niacinamide 0.45g, phytic acid
30 μ L, immobilization complex enzyme 3g, folacin coupled chitosan 0.6g, 2 μ L of benzyl alcohol-beta-glucosidase, after mixing, add water to be settled to
100mL。
The preparation process of immobilization complex enzyme are as follows: tannase plus water are configured to the tannin enzyme solution of 0.1mg/mL；By cyanine
Plain reductase adds water to be configured to the anthocyanin reductase liquid of 0.1mg/mL；By tannin enzyme solution 2.5mL, anthocyanin reductase liquid
2.5mL mixing, is added the sodium alginate aqueous solution 7mL of mass fraction 3%, mixes well；Mass fraction 2.5% is then added
Glutaraldehyde fixer makes the concentration of glutaraldehyde in the solution reach 1.25wt%；After being vibrated 30 minutes with 180 revs/min, in 20
DEG C stand crosslinking 4 hours, collect reaction solution；Reaction solution is used to the calcium chloride water of No. 5 syringe needle implantation quality scores 2%
In, it is centrifuged 15 minutes with 3000 revs/min, takes bottom solid；By bottom solid with the calcium chloride solution of mass fraction 2% 2
DEG C impregnate 2 hours, with 3000 revs/min be centrifuged 15 minutes, take bottom precipitation；By bottom precipitation mass fraction 0.075%
Glutaraldehyde solution is crosslinked 3 hours at 10 DEG C, is crossed 300 mesh filter screens, is taken filter cake；Filter cake is washed with the phosphate buffer of pH7.4
Afterwards, it drains away the water, obtains the immobilization complex enzyme.
Benzyl alcohol-beta-glucosidase obtains by the following method:
(1) 20g anhydrous sodium acetate and 25g DEXTROSE ANHYDROUS are mixed, is added in 125mL acetic anhydride, in stirring condition
Under be heated to reflux 3 hours；Then stop heating, obtained solution is poured into 1000mL ice water, stir 3 hours, there is crystal analysis
Out；Supernatant liquid is poured out, is rinsed and is crystallized with ice water, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, obtains crude product；It will be thick
Product tie product again in ethanol, in 60 DEG C, absolute pressure 0.07MPa drying 5 hours, obtain pentaacetylglucose；
(2) 4.5g pentaacetylglucose and 1.24g benzyl alcohol are added in 23mL anhydrous methylene chloride, mixing is equal
It is even；0.027g boron trifluoride ether is added, after 25 DEG C are stirred to react 24 hours, collects reaction solution；Reaction solution is successively used
The sodium bicarbonate aqueous solution of 50mL mass fraction 5% is extracted twice, and is merged organic phase, is obtained extract liquor；By its etc. of extract liquor
After the saturated saline solution washing of volume, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, light yellow oil is obtained；It will
Light yellow oil silica gel column chromatography separating purification, eluent are V (chloroform): V (methanol)=15:1, then acetone recrystallization,
In 60 DEG C, absolute pressure 0.07MPa drying 4 hours, tetra-acetylated-β-benzyl alcohol glucoside is obtained；
(3) tetra-acetylated benzyl alcohol glucoside is added in triethylamine solution, obtains molar concentration 4.5mmol/L's
Solution, the triethylamine solution is by methanol: triethylamine: water is mixed to get with volume ratio 8:1:1, and it is small to be stirred to react 24 in 20 DEG C
When；After reaction, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, crude product is obtained；Crude product silica gel column chromatography is separated pure
Change, eluent is V (chloroform): V (methanol)=12:1, then acetone ties product again, in 60 DEG C, absolute pressure 0.07MPa dry 4 it is small
When, obtain benzyl alcohol-beta-glucosidase.
Folacin coupled chitosan is prepared by the following method: weighing 2.6g folic acid and 2.7g 1- (3- dimethylamino-propyl)-
3- ethyl-carbodiimide hydrochloride is dissolved in 100mL anhydrous dimethyl sulphoxide, is stirred in light protected environment in 25 DEG C with 100 revs/min
It mixes 40 minutes, obtains folic acid solution；2.6g chitosan is weighed, it is slow to be dissolved in pH4.7, molar concentration 0.2mol/L Acetic acid-sodium acetate
Solution is rushed, is stirred 20 minutes with 100 revs/min, obtains the chitosan solution of mass fraction 0.5%；Shell is added in folic acid solution
In glycan solution, it is stirred to react 16 hours with 100 revs/min；To after reaction, use the hydroxide of molar concentration 1mol/L
Sodium water solution adjusts the pH to 9 of reaction solution, is then successively dialysed 3 days with the phosphate buffer of pH7.4, distilled water, freezing is dry
It is dry, obtain the folacin coupled chitosan.
Embodiment 6
The preparation process of health care emperor's chrysanthemum tea, comprising the following steps:
Step S1 picking: emperor's daisy_petal part unfold it is straight, fickle in love scatter 90% when, both hands are held flower and are picked；
Step S2 is spread: upward by emperor's radial striations, being spread 10 hours at 30 DEG C of temperature；
Step S3 is spent only: being cleared up with the impurity that dust catcher adheres to emperor chrysanthemum surface, is then uniformly placed in stoving rack
On；
The protection of step S4 nutritional ingredient: emperor chrysanthemum is impregnated 5 minutes in nutritional ingredient protection liquid, and dipping temperature is 30 DEG C,
The solid-liquid ratio of emperor chrysanthemum and nutritional ingredient protection liquid is 1:10 (g/mL), takes out, drains；
Step S5 just dries: just dry with dryer, 40 DEG C of temperature, is dried to water content and reaches 50%, subsequent booth in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S6 dries again: carrying out multiple baking with dryer, temperature 50 C is dried to water content and reaches 20%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S7 final firing: carrying out final firing with dryer, and temperature 60 C is dried to water content and reaches 10%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes, obtains the health care emperor chrysanthemum tea.
The preparation process of the nutritional ingredient protection liquid are as follows: weigh glucolactone 0.2g, niacinamide 0.45g, phytic acid
30 μ L, immobilization complex enzyme 3g, folacin coupled chitosan 0.6g, 2 μ L of benzyl carbinol-beta-glucosidase, after mixing, add water to be settled to
100mL。
The preparation process of immobilization complex enzyme are as follows: tannase plus water are configured to the tannin enzyme solution of 0.1mg/mL；By cyanine
Plain reductase adds water to be configured to the anthocyanin reductase liquid of 0.1mg/mL；By tannin enzyme solution 2.5mL, anthocyanin reductase liquid
2.5mL mixing, is added the sodium alginate aqueous solution 7mL of mass fraction 3%, mixes well；Mass fraction 2.5% is then added
Glutaraldehyde fixer makes the concentration of glutaraldehyde in the solution reach 1.25wt%；After being vibrated 30 minutes with 180 revs/min, in 20
DEG C stand crosslinking 4 hours, collect reaction solution；Reaction solution is used to the calcium chloride water of No. 5 syringe needle implantation quality scores 2%
In, it is centrifuged 15 minutes with 3000 revs/min, takes bottom solid；By bottom solid with the calcium chloride solution of mass fraction 2% 2
DEG C impregnate 2 hours, with 3000 revs/min be centrifuged 15 minutes, take bottom precipitation；By bottom precipitation mass fraction 0.075%
Glutaraldehyde solution is crosslinked 3 hours at 10 DEG C, is crossed 300 mesh filter screens, is taken filter cake；Filter cake is washed with the phosphate buffer of pH7.4
Afterwards, it drains away the water, obtains the immobilization complex enzyme.
Benzyl carbinol-beta-glucosidase obtains by the following method:
(1) 20g anhydrous sodium acetate and 25g DEXTROSE ANHYDROUS are mixed, is added in 125mL acetic anhydride, in stirring condition
Under be heated to reflux 3 hours；Then stop heating, obtained solution is poured into 1000mL ice water, stir 3 hours, there is crystal analysis
Out；Supernatant liquid is poured out, is rinsed and is crystallized with ice water, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, obtains crude product；It will be thick
Product tie product again in ethanol, in 60 DEG C, absolute pressure 0.07MPa drying 5 hours, obtain pentaacetylglucose；
(2) 4.5g pentaacetylglucose and 1.22g 2 phenylethyl alcohol are added in 23mL anhydrous methylene chloride, are mixed
Uniformly；0.027g boron trifluoride ether is added, after 25 DEG C are stirred to react 24 hours, collects reaction solution；Reaction solution is successive
It is extracted twice with the sodium bicarbonate aqueous solution of 50mL mass fraction 5%, merges organic phase, obtain extract liquor；Extract liquor is used it
After isometric saturated saline solution washing, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, light yellow oil is obtained；
By light yellow oil silica gel column chromatography separating purification, eluent is V (chloroform): V (methanol)=15:1, then acetone is tied again
Crystalline substance obtains tetra-acetylated-bata-phenethyl alcohol glucoside in 60 DEG C, absolute pressure 0.07MPa drying 4 hours；
(3) tetra-acetylated benzyl carbinol glucoside is added in triethylamine solution, obtains molar concentration 4.5mmol/L's
Solution, the triethylamine solution is by methanol: triethylamine: water is mixed to get with volume ratio 8:1:1, and it is small to be stirred to react 24 in 20 DEG C
When；After reaction, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, crude product is obtained；Crude product silica gel column chromatography is separated pure
Change, eluent is V (chloroform): V (methanol)=12:1, then acetone ties product again, in 60 DEG C, absolute pressure 0.07MPa dry 4 it is small
When, obtain benzyl carbinol-beta-glucosidase.
Folacin coupled chitosan is prepared by the following method: weighing 2.6g folic acid and 2.7g 1- (3- dimethylamino-propyl)-
3- ethyl-carbodiimide hydrochloride is dissolved in 100mL anhydrous dimethyl sulphoxide, is stirred in light protected environment in 25 DEG C with 100 revs/min
It mixes 40 minutes, obtains folic acid solution；2.6g chitosan is weighed, it is slow to be dissolved in pH4.7, molar concentration 0.2mol/L Acetic acid-sodium acetate
Solution is rushed, is stirred 20 minutes with 100 revs/min, obtains the chitosan solution of mass fraction 0.5%；Shell is added in folic acid solution
In glycan solution, it is stirred to react 16 hours with 100 revs/min；To after reaction, use the hydroxide of molar concentration 1mol/L
Sodium water solution adjusts the pH to 9 of reaction solution, is then successively dialysed 3 days with the phosphate buffer of pH7.4, distilled water, freezing is dry
It is dry, obtain the folacin coupled chitosan.
Embodiment 7
The preparation process of health care emperor's chrysanthemum tea, comprising the following steps:
Step S1 picking: emperor's daisy_petal part unfold it is straight, fickle in love scatter 90% when, both hands are held flower and are picked；
Step S2 is spread: with dust catcher by emperor's radial striations upward, spread 10 hours at 30 DEG C of temperature；
Step S3 is spent only: being cleared up the impurity of emperor chrysanthemum surface attachment, is then uniformly placed on stoving rack；
The protection of step S4 nutritional ingredient: emperor chrysanthemum is impregnated 5 minutes in nutritional ingredient protection liquid, and dipping temperature is 30 DEG C,
The solid-liquid ratio of emperor chrysanthemum and nutritional ingredient protection liquid is 1:10 (g/mL), takes out, drains；
Step S5 just dries: just dry with dryer, 40 DEG C of temperature, is dried to water content and reaches 50%, subsequent booth in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S6 dries again: carrying out multiple baking with dryer, temperature 50 C is dried to water content and reaches 20%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes；
Step S7 final firing: carrying out final firing with dryer, and temperature 60 C is dried to water content and reaches 10%, then spreads out in time
It dries in the air, 30 DEG C of airing temperature, the airing time 90 minutes, obtains the health care emperor chrysanthemum tea.
The preparation process of the nutritional ingredient protection liquid are as follows: weigh glucolactone 0.2g, niacinamide 0.45g, phytic acid
30 μ L, immobilization complex enzyme 3g, folacin coupled chitosan 0.6g, 1 μ L of benzyl alcohol-beta-glucosidase, benzyl carbinol-beta-glucosidase
1 μ L, after mixing, adds water to be settled to 100mL.
The preparation process of immobilization complex enzyme are as follows: tannase plus water are configured to the tannin enzyme solution of 0.1mg/mL；By cyanine
Plain reductase adds water to be configured to the anthocyanin reductase liquid of 0.1mg/mL；By tannin enzyme solution 2.5mL, anthocyanin reductase liquid
2.5mL mixing, is added the sodium alginate aqueous solution 7mL of mass fraction 3%, mixes well；Mass fraction 2.5% is then added
Glutaraldehyde fixer makes the concentration of glutaraldehyde in the solution reach 1.25wt%；After being vibrated 30 minutes with 180 revs/min, in 20
DEG C stand crosslinking 4 hours, collect reaction solution；Reaction solution is used to the calcium chloride water of No. 5 syringe needle implantation quality scores 2%
In, it is centrifuged 15 minutes with 3000 revs/min, takes bottom solid；By bottom solid with the calcium chloride solution of mass fraction 2% 2
DEG C impregnate 2 hours, with 3000 revs/min be centrifuged 15 minutes, take bottom precipitation；By bottom precipitation mass fraction 0.075%
Glutaraldehyde solution is crosslinked 3 hours at 10 DEG C, is crossed 300 mesh filter screens, is taken filter cake；Filter cake is washed with the phosphate buffer of pH7.4
Afterwards, it drains away the water, obtains the immobilization complex enzyme.
Benzyl alcohol-beta-glucosidase obtains by the following method:
(1) 20g anhydrous sodium acetate and 25g DEXTROSE ANHYDROUS are mixed, is added in 125mL acetic anhydride, in stirring condition
Under be heated to reflux 3 hours；Then stop heating, obtained solution is poured into 1000mL ice water, stir 3 hours, there is crystal analysis
Out；Supernatant liquid is poured out, is rinsed and is crystallized with ice water, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, obtains crude product；It will be thick
Product tie product again in ethanol, in 60 DEG C, absolute pressure 0.07MPa drying 5 hours, obtain pentaacetylglucose；
(2) 4.5g pentaacetylglucose and 1.24g benzyl alcohol are added in 23mL anhydrous methylene chloride, mixing is equal
It is even；0.027g boron trifluoride ether is added, after 25 DEG C are stirred to react 24 hours, collects reaction solution；Reaction solution is successively used
The sodium bicarbonate aqueous solution of 50mL mass fraction 5% is extracted twice, and is merged organic phase, is obtained extract liquor；By its etc. of extract liquor
After the saturated saline solution washing of volume, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, light yellow oil is obtained；It will
Light yellow oil silica gel column chromatography separating purification, eluent are V (chloroform): V (methanol)=15:1, then acetone recrystallization,
In 60 DEG C, absolute pressure 0.07MPa drying 4 hours, tetra-acetylated-β-benzyl alcohol glucoside is obtained；
(3) tetra-acetylated benzyl alcohol glucoside is added in triethylamine solution, obtains molar concentration 4.5mmol/L's
Solution, the triethylamine solution is by methanol: triethylamine: water is mixed to get with volume ratio 8:1:1, and it is small to be stirred to react 24 in 20 DEG C
When；After reaction, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, crude product is obtained；Crude product silica gel column chromatography is separated pure
Change, eluent is V (chloroform): V (methanol)=12:1, then acetone ties product again, in 60 DEG C, absolute pressure 0.07MPa dry 4 it is small
When, obtain benzyl alcohol-beta-glucosidase.
Benzyl carbinol-beta-glucosidase obtains by the following method:
(1) 20g anhydrous sodium acetate and 25g DEXTROSE ANHYDROUS are mixed, is added in 125mL acetic anhydride, in stirring condition
Under be heated to reflux 3 hours；Then stop heating, obtained solution is poured into 1000mL ice water, stir 3 hours, there is crystal analysis
Out；Supernatant liquid is poured out, is rinsed and is crystallized with ice water, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, obtains crude product；It will be thick
Product tie product again in ethanol, in 60 DEG C, absolute pressure 0.07MPa drying 5 hours, obtain pentaacetylglucose；
(2) 4.5g pentaacetylglucose and 1.22g 2 phenylethyl alcohol are added in 23mL anhydrous methylene chloride, are mixed
Uniformly；0.027g boron trifluoride ether is added, after 25 DEG C are stirred to react 24 hours, collects reaction solution；Reaction solution is successive
It is extracted twice with the sodium bicarbonate aqueous solution of 50mL mass fraction 5%, merges organic phase, obtain extract liquor；Extract liquor is used it
After isometric saturated saline solution washing, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, light yellow oil is obtained；
By light yellow oil silica gel column chromatography separating purification, eluent is V (chloroform): V (methanol)=15:1, then acetone is tied again
Crystalline substance obtains tetra-acetylated-bata-phenethyl alcohol glucoside in 60 DEG C, absolute pressure 0.07MPa drying 4 hours；
(3) tetra-acetylated benzyl carbinol glucoside is added in triethylamine solution, obtains molar concentration 4.5mmol/L's
Solution, the triethylamine solution is by methanol: triethylamine: water is mixed to get with volume ratio 8:1:1, and it is small to be stirred to react 24 in 20 DEG C
When；After reaction, in 60 DEG C, absolute pressure 0.07MPa drying 8 hours, crude product is obtained；Crude product silica gel column chromatography is separated pure
Change, eluent is V (chloroform): V (methanol)=12:1, then acetone ties product again, in 60 DEG C, absolute pressure 0.07MPa dry 4 it is small
When, obtain benzyl carbinol-beta-glucosidase.
Folacin coupled chitosan is prepared by the following method: weighing 2.6g folic acid and 2.7g 1- (3- dimethylamino-propyl)-
3- ethyl-carbodiimide hydrochloride is dissolved in 100mL anhydrous dimethyl sulphoxide, is stirred in light protected environment in 25 DEG C with 100 revs/min
It mixes 40 minutes, obtains folic acid solution；2.6g chitosan is weighed, it is slow to be dissolved in pH4.7, molar concentration 0.2mol/L Acetic acid-sodium acetate
Solution is rushed, is stirred 20 minutes with 100 revs/min, obtains the chitosan solution of mass fraction 0.5%；Shell is added in folic acid solution
In glycan solution, it is stirred to react 16 hours with 100 revs/min；To after reaction, use the hydroxide of molar concentration 1mol/L
Sodium water solution adjusts the pH to 9 of reaction solution, is then successively dialysed 3 days with the phosphate buffer of pH7.4, distilled water, freezing is dry
It is dry, obtain the folacin coupled chitosan.
Effect example 1
The active component content of Examples 1 to 7 health care emperor's chrysanthemum tea is measured.
Chrysanthemum contains there are many chemical component, and wherein Flavonoid substances are considered as wherein most functional materials of effect,
With dispelling wind, the effect of heat-clearing, improving eyesight, removing toxic substances.Clinically it is usually used in treating high blood pressure and coronary heart disease.
Flavone compound is many kinds of in chrysanthemum, luteolin and luteolin -7-o- β-D glucoside be chrysanthemum most
For one of main Flavonoid substances, the main indicator of chrysanthemum beverage quality and color is even more evaluated.
The preparation of the sample solution to be tested: strong emperor's chrysanthemum tea of going bail for crushed 0.25mm sieve, solid-liquid ratio 1:40 (g/mL), extraction temperature
90 DEG C, extraction time 30 minutes；It after the completion of extraction, is filtered while hot with absorbent cotton, is then filtered, filtered with double-round qualitative filter paper
Liquid, as the sample solution to be tested.
Luteolin and luteolin -7-o- β-D glucoside standard sample are purchased from Changsha Xiang Yu Biotechnology Co., Ltd.
Luteolin and luteolin -7-o- β-D glucoside are measured using high performance liquid chromatography, and determination condition is such as
Under:
Test equipment: Shimadzu LC-2010A type high performance liquid chromatograph；
Chromatographic column: Shimadzu Shim-pack CLC-ODS column (6.0mm × 150mm, 5 μm)；
Detection wavelength: 350nm；
Sample volume: 10 μ L；
Column temperature: 28 DEG C；
Mobile phase: mobile phase A is acetic acid: acetonitrile: water=0.5:3:96.5 (v/v/v)；Mobile phase B is acetic acid: acetonitrile: water
=0.5:30:69.5 (v/v/v)；B phase is by 30% (V) to 100% (V), elution time 45min；
Flow velocity: 1.0mL/min.
Specific test result is shown in Table 1.
1 content determinations of active component result table of table
As known from Table 1, by the present invention in that it is special with glucolactone, immobilised enzymes, niacinamide, phytic acid and chitosan etc.
Obtained nutritional ingredient protection liquid is formed calmly, plays good antioxidation.The preparation process of health care emperor chrysanthemum tea of the present invention
In, not only avoiding steaming step using high temperature prevents from destroying chrysanthemum effective component, but also protects liquid processing by nutritional ingredient, anti-
Only the especially Flavonoid substances of the active constituent in chrysanthemum are oxidized destruction, play a very good protection.
Effect example 2
The color lightness of Examples 1 to 7 health care emperor's chrysanthemum tea is measured.
The preparation of the sample solution to be tested: strong emperor's chrysanthemum tea of going bail for crushed 0.25mm sieve, solid-liquid ratio 1:40 (g/mL), extraction temperature
90 DEG C, extraction time 30 minutes；It after the completion of extraction, is filtered while hot with absorbent cotton, is then filtered, filtered with double-round qualitative filter paper
Liquid, as the sample solution to be tested.
The soup look of the sample solution to be tested uses Ao Yike TCP2-AE colour difference meter (offer of Beijing Ao Yike photoelectric instrument Co., Ltd)
Brightness value is measured, using distilled water as control.
Lightness difference " Δ L " value is sample brightness value and compare the difference between distilled water brightness value.Lightness difference is bigger
Illustrate that sample is limpider.
Specific test result is shown in Table 2.
2 color lightness measurement result table of table
| ΔL | |
| Embodiment 1 | -9.42 |
| Embodiment 2 | -8.37 |
| Embodiment 3 | -7.12 |
| Embodiment 4 | -6.09 |
| Embodiment 5 | -5.27 |
| Embodiment 6 | -4.96 |
| Embodiment 7 | -4.35 |
There is presently no existing standards to evaluate the quality of chrysanthemum tea and the degree of correlation of color.But chrysanthemum tea-drinking
Consumer's majority focus on chrysanthemum tea-drinking transparency.Chrysanthemum tea-drinking is easy to happen brown stain, trace it to its cause be because, chrysanthemum it is interior
It is easy to be influenced by light, heat, oxygen, acid, alkali etc. containing substance, so that its internal substance aoxidizes, and then affects millet paste
Color.It is obtained in the present invention by using specific compositions such as glucolactone, immobilised enzymes, niacinamide, phytic acid and chitosans
Nutritional ingredient protect liquid, slow down the oxidation of Flavonoid substances, ensure that the stability of chrysanthemum tea, so that the present invention obtained
Health care emperor's chrysanthemum tea has good lightness and color.
Effect example 3
The solid content of Examples 1 to 7 health care emperor's chrysanthemum tea is measured.
The preparation of the sample solution to be tested: strong emperor's chrysanthemum tea of going bail for crushed 0.25mm sieve, solid-liquid ratio 1:40 (g/mL), extraction temperature
90 DEG C, extraction time 30 minutes；It after the completion of extraction, is filtered while hot with absorbent cotton, is then filtered, filtered with double-round qualitative filter paper
Liquid, as the sample solution to be tested.
Solid content is measured referring to " tea divides determination of extractives " GB/T 8305-2002.
Specific test result is shown in Table 3.
3 solid content measurement result table of table
Effect example 4
The subjective appreciation group for selecting 10 trained Majors of Food compositions of personnel, according to the evaluation criteria pair of table 4
Examples 1 to 7 health care emperor's chrysanthemum tea carries out organoleptic properties evaluation.
4 evaluation criteria of table
As a result, it has been found that the subjective appreciation total score of Examples 1 to 7 reaches 70 points or more, the wherein total score of embodiment 4~7
Reach 80 points or more.
It should be appreciated that although this specification is described in terms of embodiments, but not each embodiment only includes one
A independent technical solution, for the sake of this narrating mode of specification is used for the purpose of clearly, those skilled in the art should be incited somebody to action
As a whole, the technical solutions in the various embodiments may also be suitably combined for specification, and forming those skilled in the art can
With the other embodiments of understanding.
Claims (9)
1. the preparation process of health care emperor's chrysanthemum tea, which comprises the following steps: pick, spread, spending only, just drying, drying again,
Final firing.
2. the preparation process of health care emperor chrysanthemum tea according to claim 1, which comprises the following steps:
Step S1 picking: emperor's daisy_petal part unfold it is straight, fickle in love scatter 80~90% when, both hands are held flower and are picked；
Step S2 is spread: upward by emperor's radial striations, being spread 10~15 hours at 20~35 DEG C of temperature；
Step S3 is spent only: being cleared up the impurity of emperor chrysanthemum surface attachment, is then uniformly placed on stoving rack；
Step S4 just dries: just dry with dryer, 40~45 DEG C of temperature, be dried to water content and reach 40~50%, it is subsequent and
When airing, 20~35 DEG C of airing temperature, the airing time 60~90 minutes；
Step S5 dries again: carry out multiple baking with dryer, 45~50 DEG C of temperature, be dried to water content and reach 15~20%, then and
When airing, 20~35 DEG C of airing temperature, the airing time 60~90 minutes；
Step S6 final firing: carrying out final firing with dryer, 60~65 DEG C of temperature, be dried to water content and reach 9~10%, then in time
Airing, the airing time 80~100 minutes, obtains the health care emperor chrysanthemum tea by 20~35 DEG C of airing temperature.
3. the preparation process of health care emperor chrysanthemum tea according to claim 1, which comprises the following steps:
Step S1 picking: emperor's daisy_petal part unfold it is straight, fickle in love scatter 80~90% when, both hands are held flower and are picked；
Step S2 is spread: upward by emperor's radial striations, being spread 10~15 hours at 20~35 DEG C of temperature；
Step S3 is spent only: being cleared up the impurity of emperor chrysanthemum surface attachment, is then uniformly placed on stoving rack；
The protection of step S4 nutritional ingredient: emperor chrysanthemum is impregnated 5~10 minutes in nutritional ingredient protection liquid, takes out, drains；
Step S5 just dries: just dry with dryer, 40~45 DEG C of temperature, be dried to water content and reach 40~50%, it is subsequent and
When airing, 20~35 DEG C of airing temperature, the airing time 60~90 minutes；
Step S6 dries again: carry out multiple baking with dryer, 45~50 DEG C of temperature, be dried to water content and reach 15~20%, then and
When airing, 20~35 DEG C of airing temperature, the airing time 60~90 minutes；
Step S7 final firing: carrying out final firing with dryer, 60~65 DEG C of temperature, be dried to water content and reach 9~10%, then in time
Airing, the airing time 80~100 minutes, obtains the health care emperor chrysanthemum tea by 20~35 DEG C of airing temperature.
4. the preparation process of health care emperor chrysanthemum tea according to claim 3, which is characterized in that the nutritional ingredient protection liquid
Preparation process are as follows: weigh 0.2~0.3g of glucolactone, 0.4~0.45g of niacinamide, 20~50 μ L of phytic acid, immobilised enzymes 3
~5g, 1~2g of chitosan, after mixing, add water to be settled to 100mL.
5. the preparation process of health care emperor chrysanthemum tea according to claim 3, which is characterized in that the nutritional ingredient protection liquid
Preparation process are as follows: weigh 0.2~0.3g of glucolactone, 0.4~0.45g of niacinamide, 20~50 μ L of phytic acid, immobilised enzymes 3
~5g, 0.3~0.6g of chitosan, 1~3 μ L of aromatic alkyl glucoside, after mixing, add water to be settled to 100mL.
6. the preparation process of health care emperor chrysanthemum tea according to claim 3, which is characterized in that the nutritional ingredient protection liquid
Preparation process are as follows: weigh 0.2~0.3g of glucolactone, 0.4~0.45g of niacinamide, 20~50 μ L of phytic acid, immobilised enzymes 3
~5g, 0.3~0.6g of folacin coupled chitosan, 1~3 μ L of aromatic alkyl glucoside, after mixing, add water to be settled to 100mL.
7. the preparation process of health care emperor chrysanthemum tea according to claim 5, which is characterized in that the aromatic alkyl glucoside
For benzyl alcohol-beta-glucosidase and/or benzyl carbinol-β-D glucoside.
8. the preparation process of health care emperor chrysanthemum tea according to claim 6, which is characterized in that the folacin coupled chitosan is logical
It crosses following methods preparation: weighing 2.6~2.8g folic acid and 2.6~2.8g 1- (3- dimethylamino-propyl) -3- ethyl carbodiimide
Hydrochloride is dissolved in 100~150mL anhydrous dimethyl sulphoxide, is stirred 40~60 minutes, is obtained in 20~30 DEG C in light protected environment
Folic acid solution；2.6~2.8g chitosan is weighed, pH4.7, molar concentration 0.2mol/L NaAc_HAc buffer solution is dissolved in, stirs
It mixes 10~20 minutes, obtains the chitosan solution of mass fraction 0.3~0.5%；Folic acid solution is added in chitosan solution, is stirred
Mix reaction 12~16 hours；It is then successively slow with the phosphate of pH7.4 to after reaction, adjust the pH to 8~9 of reaction solution
Fliud flushing, distilled water are dialysed 3~4 days, and freeze-drying obtains the folacin coupled chitosan.
9. health care emperor's chrysanthemum tea, which is characterized in that the preparation work of health care emperor chrysanthemum tea described according to claim 1~any one of 8
Skill processes to obtain.
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