CN107375537A - The preparation method of Tea Polyphenols in southwestern camellia - Google Patents
The preparation method of Tea Polyphenols in southwestern camellia Download PDFInfo
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- CN107375537A CN107375537A CN201710612581.8A CN201710612581A CN107375537A CN 107375537 A CN107375537 A CN 107375537A CN 201710612581 A CN201710612581 A CN 201710612581A CN 107375537 A CN107375537 A CN 107375537A
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- camellia
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- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 75
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 75
- 235000018597 common camellia Nutrition 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 240000001548 Camellia japonica Species 0.000 title claims description 59
- 239000011347 resin Substances 0.000 claims abstract description 49
- 229920005989 resin Polymers 0.000 claims abstract description 49
- 238000000605 extraction Methods 0.000 claims abstract description 46
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000010828 elution Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000012535 impurity Substances 0.000 claims abstract description 12
- 238000001179 sorption measurement Methods 0.000 claims abstract description 12
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000004821 distillation Methods 0.000 claims abstract description 5
- 238000010992 reflux Methods 0.000 claims abstract description 5
- 239000012141 concentrate Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 claims description 10
- 238000002474 experimental method Methods 0.000 claims description 8
- 239000003480 eluent Substances 0.000 claims description 7
- 239000012488 sample solution Substances 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 abstract description 10
- 241000209507 Camellia Species 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 230000002745 absorbent Effects 0.000 description 5
- 239000002250 absorbent Substances 0.000 description 5
- 240000001238 Gaultheria procumbens Species 0.000 description 4
- 235000007297 Gaultheria procumbens Nutrition 0.000 description 4
- 235000010394 Solidago odora Nutrition 0.000 description 4
- 241001122767 Theaceae Species 0.000 description 4
- 230000003068 static effect Effects 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 208000006820 Arthralgia Diseases 0.000 description 1
- 241001343472 Camellia pitardii Species 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 208000005577 Gastroenteritis Diseases 0.000 description 1
- 208000037093 Menstruation Disturbances Diseases 0.000 description 1
- 206010027339 Menstruation irregular Diseases 0.000 description 1
- 208000002193 Pain Diseases 0.000 description 1
- 208000012287 Prolapse Diseases 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 208000012873 acute gastroenteritis Diseases 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003266 anti-allergic effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 210000000436 anus Anatomy 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 filtering Substances 0.000 description 1
- 208000035861 hematochezia Diseases 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 201000005630 leukorrhea Diseases 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 206010046901 vaginal discharge Diseases 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/82—Theaceae (Tea family), e.g. camellia
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
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- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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- Veterinary Medicine (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Pyrane Compounds (AREA)
Abstract
The present invention provides a kind of preparation method of Tea Polyphenols in southwestern camellia, this method is using dry southwestern camellia as raw material, refluxing extraction is carried out by solvent of 50~80% aqueous acetone solution, extract solution turns to be dissolved in water, filtering after being concentrated and dried, filtrate is after DM130 macroporous resin adsorptions, with distillation water elution impurity, then elutes by 20~60% ethanol solutions of concentration, gather ethanol and take off liquid, the Tea Polyphenols product of southwestern camellia is obtained after concentrate drying.Preparation method of the present invention can total polyphenols effectively in the camellia of Extraction and enrichment southwest, the total polyphenols purity of production is high, quality is good, can be effectively protected the Nomenclature Composition and Structure of Complexes of polyphenol component; simple to operate, cost is low, uses solvent to reclaim; macroreticular resin is renewable, suitable for large-scale production.
Description
Technical field
The present invention relates to the preparation method of active component in the camellia of natural drug southwest, tea in specifically southwestern camellia
The preparation method of polyphenol.
Background technology
Southwestern camellia (Camellia pitardii), alias southwest Camellia, is the evergreen evergreen shrubs of Camellia or little Qiao
Wood, originate in the provinces and regions such as China Hunan, Guangxi, Yunnan, Guizhou and Sichuan.Southwestern camellia has promoting blood circulation and hemostasis, astringing to arrest diarrhea, and removing toxic substances is held back
Sore and other effects, irregular menstruation is cured mainly, menorrhalgia, discharging fresh blood stool, is spitted blood, acute gastroenteritis, dysentery, prolapse of the anus, leukorrhea, seminal emission,
Arthralgia pain due to rheumatism, burn, scald etc..The Tea Polyphenols system representativeness that enriching and purifying obtains in the camellia of South Mountain westerly is more in southwestern camellia
Phenols component.Modern pharmacology research shows that southwestern camellia has the pharmacological activities such as anti-inflammatory, antiallergy.
Therefore, the further investigation to tea polyphenol extract purification enrichment technique in southwestern camellia is necessary, and right at present
In southwestern camellia the process of enriching of Tea Polyphenols study less and traditional process majority will be by soda acid, enzyme, super
The processing such as sound, can influence the Nomenclature Composition and Structure of Complexes of total polyphenols, and the yield of extract is low, and impurity is more, be brought to subsequent treatment work
Very big difficulty, wastes time and energy, and is unfavorable for the development and utilization of southwestern camellia medical value.
The content of the invention
It is an object of the invention to overcome the shortcomings of conventional art, there is provided Tea Polyphenols in a kind of camellia of high-purity southwest
Enriching and purifying preparation method.
For achieving the above object, the present invention uses following technical scheme：
The preparation method of Tea Polyphenols, comprises the following steps in southwestern camellia：
(1) dried southwestern camellia raw material is crushed；
(2) using 50~80% acetone-water solution as solvent, southwestern camellia presses solid-liquid ratio (g with Extraction solvent:ml)
For 1:Southwestern camellia in 10~40 refluxing extraction steps (1)；Extracting temperature is 60~100 DEG C, and extraction time is 1~5h,
Extraction time is 1~4 time, merges extract solution；
(3) total polyphenols yield highest extract solution is filtered out by experiment of single factor and orthogonal test；
(4) turn to be dissolved in water, filtering after extract solution in step (3) is concentrated and dried；
(5) filtrate is miscellaneous with the distillation water elution impurity of 3~5 times of amount of resin (ml/g) after DM130 macroporous resin adsorptions
After matter elution completely, then eluted as 20~60% ethanol solutions using the concentration of 12~21 times of amount of resin (ml/g), collection eluent；
(6) Determination of Polyphenols highest eluent is filtered out by experiment of single factor；
(7) eluent obtained in step (6) is concentrated and dried, produces the Tea Polyphenols product of southwestern camellia.
In preferred steps (2) Extraction solvent be concentration be 50% acetone-water solution, solid-liquid ratio (g:Ml it is) 1:40, carry
It is 70 DEG C, extraction time 3h to take temperature, and extraction time is 2 times.
Filtrate is after DM130 macroporous resin adsorptions in preferred steps (5), with the distillation water elution of 3 times of amount of resin (ml/g)
Impurity, then eluted by 30% ethanol solution of the concentration of 13.5 times of amount of resin (ml/g), collect ethanol eluate.
The amount of load solution is 3 times of amount of resin (ml/g) in above-mentioned steps (5).
Further, in above-mentioned southwestern camellia Tea Polyphenols preparation method, comprise the following steps：
(1) dried southwestern camellia raw material is crushed；
(2) using 50% acetone-water solution as Extraction solvent, southwestern camellia presses solid-liquid ratio (g with Extraction solvent:Ml)=
1:Southwestern camellia in 40 refluxing extraction steps (1)；Extracting temperature is 70 DEG C, is extracted 2 times, each 3h, merges extract solution；
(3) turn to be dissolved in water and filter after extract solution is concentrated and dried；
(4) filtrate distills water elution impurity after DM130 macroporous resin adsorptions with 3 times of amount of resin (ml/g), then with 13.5
The concentration of times amount of resin (ml/g) is the elution of 30% ethanol solution, collects ethanol eluate, southwestern camellia is produced after concentrate drying
Colored Tea Polyphenols product.
Load solution polyphenol content is 110.66mg/ml in above-mentioned steps (4).
Compared with prior art, the beneficial effects of the invention are as follows：The preparation method overcomes traditional handicraft southwest camellia
The deficiency that middle Tea Polyphenols is easy to run off, yield is low and purity is not high, improve the efficiency of tea polyphenol extract in southwestern camellia and obtain
Rate, total polyphenols composition composition, structure and activity effectively being protected, the maximum amount of efficiently production, purity is high, and simple to operate,
Cost is low, and acetone, ethanol equal solvent can reclaim, and macroreticular resin is renewable, suitable for large-scale production.
Brief description of the drawings
Fig. 1：The preparation method flow chart of Tea Polyphenols in the southwestern camellia of embodiment.
Embodiment
With specific embodiment, the present invention will be further described below, unless otherwise specified, in the embodiment
Developed the color using P-Mo-Wo acid-sodium carbonate, the content of Tea Polyphenols in the camellia of spectrophotometry southwest.
The embodiment of the preparation method of Tea Polyphenols is in the southwestern camellia of the present invention：With dry southwestern camellia
Flower for raw material carry out solvent extraction, Extraction solvent be 50~80% acetone-water solution, solid-liquid ratio (g：Ml)=1:10~40,
Extracting temperature is 60~100 DEG C, and extraction time is 1~5h, and extraction time is 1~4 time；Extract turns to be dissolved in after being concentrated and dried
Water, filtering, filtrate distills water elution impurity after DM130 macroporous resin adsorptions, with 3~5 times of amount of resin (ml/g), finally with 12
The concentration of~21 times of amount of resin (ml/g) elutes for 20~60% ethanol solutions, gathers last part eluent, is concentrated and dried
Afterwards southwestern camellia Tea Polyphenols product.
The extraction to Tea Polyphenols in southwestern camellia and purifying resin step are described in detail below.
First, process for extracting tea polyphenol embodiment in southwestern camellia
The yield calculating formula of product Tea Polyphenols is as follows：
The content of the yield of southwestern camellia total polyphenols=southwestern camellia total polyphenols × extraction medicinal extract amount ÷ material quantity × 100%
Embodiment 1~4
This part embodiment is the influence for investigating Extraction solvent concentration to the yield of Tea Polyphenols in southwestern camellia.Specific bar
Part is set and experimental result is shown in Table 1：
Table 1
The yield highest of total polyphenols when acetone concentration is 50%, but continue to increase with acetone concentration, the receipts of total polyphenols
Rate substantially reduces, it may be possible to due to the original that 50% aqueous acetone solution is good to total polyphenols solubility property, the swelling coefficient to raw material is high
Cause.So it is 50% acetone-water to select Extraction solvent.
Embodiment 5~9
This part embodiment is the influence for investigating extraction time to the yield of Tea Polyphenols in southwestern camellia.Actual conditions is set
Fixed and experimental result is shown in Table 2：
Table 2
Total polyphenols yield highest when extraction time is 4h, with the extension of extraction time, the yield of total polyphenols is
Decline, therefore be chosen to be 4 hours optimum extraction time.
Embodiment 10~14
This part embodiment is the influence for investigating Extracting temperature to the yield of Tea Polyphenols in southwestern camellia.Actual conditions is set
Fixed and experimental result is shown in Table 3：
Table 3
Total polyphenols yield increases with the rise of Extracting temperature, but temperature is higher than 70 DEG C, and Determination of Polyphenols is decreased obviously.Cause
This, is chosen to be 70 DEG C of optimum extraction temperature.
Embodiment 15~21
This part embodiment is the influence for investigating solid-liquid ratio to the yield of Tea Polyphenols in southwestern camellia.Actual conditions is set
And experimental result is shown in Table 4：
Table 4
The yield of total polyphenols is 1 in solid-liquid ratio:Peaked when 35, therefore selected solid-liquid ratio is 1:35.
Embodiment 22~25
This part embodiment is the influence for investigating extraction time to the yield of Tea Polyphenols in southwestern camellia.Actual conditions is set
Fixed and experimental result is shown in Table 5：
Table 5
With the increase of extraction time, the yield of southwestern camellia total polyphenols increased, but more than 2 times after, its it is increased become
Gesture is gradually delayed.Energy consumption can be increased in view of increase extraction time, and 2 extraction cans substantially extract southwestern camellia total polyphenols
Completely.Therefore extraction time is set as 2 times.
Embodiment 26
The present embodiment is the orthogonal experiment for investigating extraction process, according to the result of previous embodiment 1~25, to four factors
3 suitable levels are selected respectively, using L9(34) orthogonal experiment calendar investigation optimum process condition.Orthogonal test factor water
Safety row is shown in Table 6, and experimental result is shown in Table 7：
Table 6
Table 7
From analysis of experimental results, the influence of each factor is followed successively by B>C>A>D, i.e. extraction time>Extracting temperature>Extraction
Solvent strength>Extraction solvent is measured again；A2B3C1D2With A2B1C2D3Process combination it is ideal, and both combination total polyphenols
Content and yield are closer to, so in order to reduce the production cost of enterprise, production efficiency are improved, so optimised process is combined as
A2B1C2D3.50% acetone-water of i.e. 40 times amounts, 70 DEG C, extract 2 times, 3 hours every time, Determination of Polyphenols 41.41% was total more
The yield of phenol is 15.36%.Wherein extraction time has a great influence to total polyphenols extraction.
2nd, in the camellia of DM130 types macroporous resin purification southwest total polyphenols process example
Pre-processed before the use of DM130 type macroreticular resins and reclaim post-processing step, specific preprocess method is as follows：Carrying
Take in device, add the ethanol immersion 2-4h higher than resin bed 10-20cm, then put net cleaning solution.Outlet is washed till repeatedly with same method
Cleaning solution is in test tube plus untill 3 times of amount water are not aobvious muddy, after fully eluted with distilled water untill without obvious ethanol smell, i.e.,
It can be used.
To optimize the use of resin, the present embodiment is investigated to resin property parameter first, and detailed process is as follows：
1. the determination of dynamic adsorbance
DM130 type macroporous absorbent resins 20g is taken to fill post (blade diameter length ratio 1：10), sample solution is continuous with 2BV/h flow velocity
By resin column, efflux is collected, determines the concentration of efflux Chinese and Western South Mountain tea total polyphenols, it is always more with efflux Chinese and Western South Mountain tea
The concentration (mg/mL) of phenol is ordinate, and the volume (mL) of sample solution is abscissa, draws adsorption curve.8 are the results are shown in Table, when
When the volume of sample solution adds to 210mL, DM130 type macroporous absorbent resins reach saturation.
The Dynamic Adsorption of the southwestern camellia total polyphenols of table 8
2. the determination of static adsorbance
The DM130 type macroporous absorbent resins of 10mL (being approximately equivalent to dried resin 3g) pretreatments are added in 100mL conical flasks
And 100mL sample solutions.Shaken at room temperature 3 hours, the content of determination sample solution Chinese and Western South Mountain tea total polyphenols is taken out, according to following formula
Calculate static adsorbance q=(C during material balance0- C) V/G, the static capacity for learning DM130 type macroreticular resins is per g
Macroporous resin adsorption 87.0mg polyphenol, C in formula0It is respectively the initial concentration with solution Chinese and Western South Mountain tea total polyphenols during balance with C
(mg/mL), V is test liquid volume (mL), and G is amount of resin (g).
Embodiment 27~31
This part embodiment is to investigate DM130 type macroporous absorbent resin ethanol elution concentration.Actual conditions is set and experiment
It the results are shown in Table 9：
Table 9
With the increase of concentration of alcohol, the purity and eluting rate of total polyphenols reduce, in order to improve the content of total polyphenols and wash
De- rate, selects 30% ethanol to be eluted.As a result the content of total polyphenols and eluting rate are respectively increased to 85.27% and 21.91%.
Show to use water, 30% ethanol elution instead, the purity and eluting rate of total polyphenols all increase.
Embodiment 32~40
This part embodiment is to investigate DM130 type macroporous absorbent resin eluting agents.Actual conditions is set and experiment knot
Fruit is shown in Table 10：
Table 10
Water-solubility impurity, 30% second of 13.5 times of weight resins can be just removed substantially with the deionized water of 3 times of weight resins
Alcohol elution substantially can elute total polyphenols completely, therefore the dosage of determination deionized water is 3 times of weight resins, and 30% ethanol is washed
De- liquid dosage is 13.5 times of weight resins.
Embodiment 41
The present embodiment technological process is as shown in Figure 1
1. crush dried southwestern camellia raw material；
2. using concentration be 50% acetone-water solution as Extraction solvent, solid-liquid ratio (g：Ml)=1:40, Extracting temperature 70
DEG C, extract 2 times, each 3h method is extracted；
3. extract solution turns to be dissolved in water and filter after being concentrated and dried, this part Determination of Polyphenols is 41.41%；
4. filtrate is through DM130 macroporous resin adsorptions, applied sample amount is 3 times of amount of resin (ml/g), afterwards with 3 times of amount of resin (ml/
G) water elution impurity is distilled, is finally eluted using the concentration of 13.5 times of amount of resin (ml/g) as 30% ethanol solution, gathers last
Elution fractions, the Tea Polyphenols product of southwestern camellia is obtained after concentrate drying, the purity of gained total polyphenols is 85.27%.
Claims (6)
1. the preparation method of Tea Polyphenols in southwestern camellia, it is characterised in that the described method comprises the following steps：
(1) dried southwestern camellia raw material is crushed；
(2) using 50~80% acetone-water solution as solvent, southwestern camellia presses solid-liquid ratio (g with Extraction solvent:Ml it is) 1:
Southwestern camellia in 10~40 refluxing extraction steps (1)；Extracting temperature is 60~100 DEG C, and extraction time is 1~5h, extraction
Number is 1~4 time, merges extract solution；
(3) total polyphenols yield highest extract solution is filtered out by experiment of single factor and orthogonal test；
(4) turn to be dissolved in water, filtering after extract solution in step (3) is concentrated and dried；
(5) filtrate is after DM130 macroporous resin adsorptions, and with the distillation water elution impurity of 3~5 times of amount of resin (ml/g), impurity is washed
It is de- completely after, then eluted as 20~60% ethanol solutions using the concentration of 12~21 times of amount of resin (ml/g), collection eluent；
(6) Determination of Polyphenols highest eluent is filtered out by experiment of single factor；
(7) eluent obtained in step (6) is concentrated and dried, produces the Tea Polyphenols product of southwestern camellia.
2. the preparation method of Tea Polyphenols in southwestern camellia according to claim 1, it is characterised in that the Extraction solvent
It is 50% acetone-water solution for concentration, solid-liquid ratio (g:Ml it is) 1:40, Extracting temperature is 70 DEG C, extraction time 3h, extraction
Number is 2 times.
3. the preparation method of Tea Polyphenols in southwestern camellia according to claim 1, it is characterised in that filtered in step (5)
Liquid is after DM130 macroporous resin adsorptions, with the distillation water elution impurity of 3 times of amount of resin (ml/g), then with 13.5 times of amount of resin
(ml/g) ethanol solution that concentration is 30% elutes, and collects ethanol eluate.
4. the preparation method of Tea Polyphenols in southwestern camellia according to claim 3, it is characterised in that in step (5)
The amount of sample solution is 3 times of amount of resin (ml/g).
5. the preparation method of Tea Polyphenols in southwestern camellia according to claim 1, it is characterised in that this method is included such as
Lower step：
(1) dried southwestern camellia raw material is crushed；
(2) using 50% acetone-water solution as Extraction solvent, southwestern camellia presses solid-liquid ratio (g with Extraction solvent:Ml)=1:40
Southwestern camellia in refluxing extraction step (1)；Extracting temperature is 70 DEG C, is extracted 2 times, each 3h, merges extract solution；
(3) turn to be dissolved in water and filter after extract solution is concentrated and dried；
(4) filtrate distills water elution impurity after DM130 macroporous resin adsorptions with 3 times of amount of resin (ml/g), then with 13.5 times of trees
The concentration of fat amount (ml/g) elutes for 30% ethanol solution, collects ethanol eluate, southwestern camellia is produced after concentrate drying
Tea Polyphenols product.
6. the preparation method of Tea Polyphenols in southwestern camellia according to claim 5, it is characterised in that the step (4)
Middle load solution polyphenol content is 110.66mg/ml.
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| CN112094828A (en) * | 2020-10-31 | 2020-12-18 | 洞口县亿丰农林牧科技有限公司 | Method for extracting SOD (superoxide dismutase) and theanine from camellia |
| CN113577165A (en) * | 2021-07-31 | 2021-11-02 | 海南黎草纪新生物科技有限公司 | Method for extracting polyphenol from camellia japonica |
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| CN103145770A (en) * | 2013-03-20 | 2013-06-12 | 宜宾学院 | Method for extracting polyphenol from camellia |
| CN106478744A (en) * | 2016-08-26 | 2017-03-08 | 潜山县妙山茶业有限公司 | A kind of technique extracting tea polyphenols from Folium Camelliae sinensis |
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| CN103145770A (en) * | 2013-03-20 | 2013-06-12 | 宜宾学院 | Method for extracting polyphenol from camellia |
| CN106478744A (en) * | 2016-08-26 | 2017-03-08 | 潜山县妙山茶业有限公司 | A kind of technique extracting tea polyphenols from Folium Camelliae sinensis |
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| CN112094828A (en) * | 2020-10-31 | 2020-12-18 | 洞口县亿丰农林牧科技有限公司 | Method for extracting SOD (superoxide dismutase) and theanine from camellia |
| CN112094828B (en) * | 2020-10-31 | 2023-07-18 | 洞口县亿丰农林牧科技有限公司 | Method for extracting SOD superoxide dismutase and theanine from camellia |
| CN113577165A (en) * | 2021-07-31 | 2021-11-02 | 海南黎草纪新生物科技有限公司 | Method for extracting polyphenol from camellia japonica |
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