CN109620864A - The mixture and its extracting method of total tannin and epicatechin and application in a kind of cymose buckwheat rhizome - Google Patents

The mixture and its extracting method of total tannin and epicatechin and application in a kind of cymose buckwheat rhizome Download PDF

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CN109620864A
CN109620864A CN201910113968.8A CN201910113968A CN109620864A CN 109620864 A CN109620864 A CN 109620864A CN 201910113968 A CN201910113968 A CN 201910113968A CN 109620864 A CN109620864 A CN 109620864A
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buckwheat rhizome
cymose buckwheat
epicatechin
mixture
extracting method
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李昌福
商国懋
吴德海
张宸
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Huayi Pharmaceutical Co Ltd
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Huayi Pharmaceutical Co Ltd
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    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • 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
    • 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
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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    • 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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Abstract

The present invention provides a kind of extracting methods of the mixture of total tannin and epicatechin in cymose buckwheat rhizome, belong to pharmaceutical preparations technology field.The temperature that the present invention passes through the smashed partial size of the specific cymose buckwheat rhizome of restriction and suspension process hot water, extract tannin and epicatechin in cymose buckwheat rhizome more complete, improve the rate of transform of active principle and the yield of Spray dried products, simultaneously by limiting specific relative density, in conjunction with the exclusive purification technique and spray drying technology of macroporous absorbent resin, keep Spray dried products form finer and smoother, good dispersion, moisture is low, the stabilized with mixture of obtained total tannin and epicatechin is good, the capsule quality of filling is good, is conducive to patient and absorbs.

Description

In a kind of cymose buckwheat rhizome the mixture and its extracting method of total tannin and epicatechin and Using
Technical field
The present invention relates to the mixing of total tannin and epicatechin in pharmaceutical preparations technology field more particularly to a kind of cymose buckwheat rhizome Object and its extracting method and application.
Background technique
Tumour (Tumor) is body under the effect of various carcinogenic factors, some cell of local organization is in gene level On lose the normal regulation grown to it, lead to its clonal abnormality hyperplasia and the neoformation that is formed.Generally tumour is divided into good Property and pernicious two major classes.All malignant tumours are collectively referred to as cancer (cancer).
Cymose buckwheat rhizome (RhizomaFagopyriCymosi) is polygonaceae plant, alias tartary buckwheat, wild bridge buckwheat, day buckwheat.Its Cool in nature, acrid flavour, hardship play the role of clearing heat and detoxicating, activating microcirculation and removing stasis medicinal, invigorating spleen to remove dampness.The extract of the drug have mitigate tumour put, Chemical therapy toxic side effect and there is synergistic effect to tumour Radiotherapy chemotherapy.
Chinese patent application CN201110369468.4 discloses the preparation process of Rhizoma Fagopyri Dibotryis extract, including following step It is rapid: to take cymose buckwheat rhizome, be ground into the particle that partial size is not more than 5mm, with ethyl alcohol heating and refluxing extraction four times, Extraction solvent quality is distinguished It is 6,4,3,2 times of cymose buckwheat rhizome granular mass, extraction time is followed successively by 90,60,60,30 minutes, combined extract, filters, filter It is 1.06~1.09 that liquid, which is concentrated under reduced pressure into relative density in 60 DEG C or less,；Add 20 times of water of medicinal extract amount, is suspended, stands overnight；Supernatant Liquid after filtering, is separated with macroporous adsorbent resin column chromatography；First be eluted with water it is colourless to efflux, after with 80% ethanol elution extremely Until eluent and ferric trichloride test solution are reactionless, 80% ethanol eluate is collected, 60 DEG C or less are concentrated under reduced pressure into relative density Be 1.06~1.09, spray drying to get.
But use Rhizoma Fagopyri Dibotryis extract there are recovery rates low, the stabilized with mixture extracted of above method preparation The problem of difference, greatly limits the curative effect of Rhizoma Fagopyri Dibotryis extract.
Summary of the invention
In consideration of it, the purpose of the present invention is to provide the mixture of total tannin in a kind of cymose buckwheat rhizome and epicatechin and its mentioning Take methods and applications.Extracting method recovery rate provided by the invention is high, the stabilized with mixture of obtained total tannin and epicatechin Property is good.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The extracting method of the mixture of total tannin and epicatechin in a kind of cymose buckwheat rhizome, comprising the following steps:
Cymose buckwheat rhizome is crushed to 2~3mm of partial size, obtains cymose buckwheat rhizome particle；
The cymose buckwheat rhizome particle is extracted with alcohol reflux, obtains extracting solution；
It is 1.06~1.09 that gained filtrate decompression after extracting solution filtering, which is concentrated into relative density, obtains medicinal extract；
Gained supernatant after filtering, is separated with macroporous adsorbent resin column chromatography after the medicinal extract is mixed with hot water, first Be eluted with water it is colourless to efflux, then with 80% ethanol elution to efflux and ferric trichloride test solution it is reactionless until, regather 80% ethyl alcohol efflux, obtains eluent, and the temperature of the hot water is 60~80 DEG C；
It is 1.02~1.04 that the eluent, which is concentrated into relative density, spray drying to get total tannin in cymose buckwheat rhizome and The mixture of epicatechin.
Preferably, the number that the alcohol reflux extracts is 4 times, ethyl alcohol and cymose buckwheat rhizome particle when the alcohol reflux extracts Mass ratio be respectively 4:1,4:1,3:1 and 1~2:1, the time that the alcohol reflux extracts is followed successively by 60,30,30 and 10min。
Preferably, the volume ratio of the medicinal extract and hot water is 1:10~20.
Preferably, the macroporous absorbent resin is D101 or AB-8.
Preferably, the partial size of the macroporous absorbent resin is 0.3~1.25mm, and specific surface area is 600~700m2/ g is put down Equal aperture is 8.5~9.5nm.
Preferably, the adsorption flow rate of the macroporous absorbent resin is 200~400L/h.
Preferably, the inlet air temperature of the spray drying is 160 DEG C~200 DEG C, and leaving air temp is 70 DEG C~100 DEG C, institute The time for stating spray drying is 6~8h.
The total tannin that is extracted from cymose buckwheat rhizome the present invention also provides the extracting method described in above-mentioned technical proposal and The mixture of epicatechin.
The present invention also provides the total tannins extracted from cymose buckwheat rhizome and epicatechin described in above-mentioned technical proposal Mixture application in preparation of anti-tumor drugs.
Preferably, the anti-tumor drug includes the mixing of the total tannin and epicatechin that extract from cymose buckwheat rhizome Object, pharmaceutically acceptable carrier and diluent.
The present invention provides a kind of extracting methods of the mixture of total tannin and epicatechin in cymose buckwheat rhizome, including following step It is rapid: cymose buckwheat rhizome being crushed to 2~3mm of partial size, obtains cymose buckwheat rhizome particle；The cymose buckwheat rhizome particle is extracted with alcohol reflux, is obtained To extracting solution；It is 1.06~1.09 that gained filtrate decompression after extracting solution filtering, which is concentrated into relative density, obtains medicinal extract；It will The medicinal extract mixed with hot water after gained supernatant after filtering, separated with macroporous adsorbent resin column chromatography, be first eluted with water to Efflux is colourless, then with 80% ethanol elution to efflux and ferric trichloride test solution it is reactionless until, regather 80% ethanol stream Liquid out, obtains eluent, and the temperature of the hot water is 60~80 DEG C；By the eluent be concentrated into relative density be 1.02~ 1.04, it is spray-dried the mixture to get total tannin in cymose buckwheat rhizome and epicatechin.The present invention is by limiting specific cymose buckwheat rhizome The temperature of hot water in smashed partial size and suspension process extracts tannin and epicatechin in cymose buckwheat rhizome more complete, The rate of transform of active principle and the yield of Spray dried products are improved, while by limiting specific relative density, in conjunction with big The exclusive purification technique and spray drying technology of macroporous adsorbent resin, keep Spray dried products form finer and smoother, good dispersion, moisture Low, the stabilized with mixture of obtained total tannin and epicatechin is good, and the capsule quality of filling is good, is conducive to patient and absorbs.
Specific embodiment
The present invention provides a kind of extracting methods of the mixture of total tannin and epicatechin in cymose buckwheat rhizome, including following step It is rapid:
Cymose buckwheat rhizome is crushed to 2~3mm of partial size, obtains cymose buckwheat rhizome particle；
The cymose buckwheat rhizome particle is extracted with alcohol reflux, obtains extracting solution；
It is 1.06~1.09 that gained filtrate decompression after extracting solution filtering, which is concentrated into relative density, obtains medicinal extract；
Gained supernatant after filtering, is separated with macroporous adsorbent resin column chromatography after the medicinal extract is mixed with hot water, first Be eluted with water it is colourless to efflux, then with 80% ethanol elution to efflux and ferric trichloride test solution it is reactionless until, regather 80% ethyl alcohol efflux, obtains eluent, and the temperature of the hot water is 60~80 DEG C；
It is 1.02~1.04 that the eluent, which is concentrated into relative density, spray drying to get total tannin in cymose buckwheat rhizome and The mixture of epicatechin.
Cymose buckwheat rhizome is crushed to 2~3mm of partial size by the present invention, obtains cymose buckwheat rhizome particle.The present invention is specific to the crushing Mode does not have special restriction, using grinding mode well known to those skilled in the art.
After obtaining cymose buckwheat rhizome particle, the present invention extracts the cymose buckwheat rhizome particle with alcohol reflux, obtains extracting solution.At this In invention, the number that the alcohol reflux extracts is preferably 4 times, the matter of ethyl alcohol and cymose buckwheat rhizome particle when the alcohol reflux extracts Amount is successively preferably 60,30,30 and than being respectively preferably 4:1,4:1,3:1 and 1~2:1, the time that the alcohol reflux extracts 10min.In the present invention, the volumetric concentration of the ethyl alcohol is preferably 93~95%.
It is 1.06 that gained filtrate decompression, which is concentrated into relative density, after obtaining extracting solution, after the present invention filters the extracting solution ~1.09 (55 DEG C), obtain medicinal extract.The present invention does not have special restriction to the concrete mode of the filtering, using art technology Filter type known to personnel.The present invention does not have special restriction to the pressure of the reduced pressure, temperature and time, adopts With mode well known to those skilled in the art.
After obtaining medicinal extract, gained supernatant after filtering, uses macroporous absorption after the present invention mixes the medicinal extract with hot water Resin column chromatography for separation, be first eluted with water it is colourless to efflux, then with 80% ethanol elution to efflux and ferric trichloride test solution Until reactionless, 80% ethyl alcohol efflux is regathered, obtains eluent, the temperature of the hot water is 60~80 DEG C.The present invention couple The mixed concrete mode does not have special restriction, using hybrid mode well known to those skilled in the art.
In the present invention, the temperature of the hot water is preferably 65~75 DEG C, and more preferably 70~72 DEG C.
In the present invention, the volume ratio of the medicinal extract and hot water is preferably 1:10~20, more preferably 1:15~18.
After mixing, the present invention preferably stands overnight mixing crude product, obtains supernatant.Tool of the present invention to the filtering Body mode does not have special restriction, using filter type well known to those skilled in the art.
In the present invention, the macroporous absorbent resin is preferably D101 or AB-8.
In the present invention, the partial size of the macroporous absorbent resin is preferably 0.3~1.25mm, and specific surface area is preferably 600 ~700m2/ g, average pore size are preferably 8.5~9.5nm.
In the present invention, the adsorption flow rate of the macroporous absorbent resin is preferably 200~400L/h, more preferably 250~ 350L/h。
After obtaining eluent, it is 1.02~1.04 (55 DEG C) that the eluent is concentrated into relative density by the present invention, spraying The dry mixture to get total tannin in cymose buckwheat rhizome and epicatechin.In the present invention, the concentration is preferably concentrated under reduced pressure, The present invention does not have special restriction to the pressure of the reduced pressure, temperature and time, and use is well known to those skilled in the art Mode.
In the present invention, the inlet air temperature of the spray drying is preferably 160 DEG C~200 DEG C, more preferably 170 DEG C~ 180 DEG C, leaving air temp is preferably 70 DEG C~100 DEG C, and more preferably 80 DEG C~90 DEG C, the time of the spray drying is preferably 6 ~8h, more preferably 7h.
The total tannin that is extracted from cymose buckwheat rhizome the present invention also provides the extracting method described in above-mentioned technical proposal and The mixture of epicatechin.
The present invention also provides the total tannins extracted from cymose buckwheat rhizome and epicatechin described in above-mentioned technical proposal Mixture application in preparation of anti-tumor drugs.
In the present invention, the anti-tumor drug preferably includes the total tannin and epicatechin extracted from cymose buckwheat rhizome Mixture, pharmaceutically acceptable carrier and diluent.
In the present invention, the dosage form of the anti-tumor drug preferably includes solid pharmaceutical preparation or liquid preparation, the solid system Agent is preferably piece, capsule, particle or pill, and the liquid preparation is preferably oral solution or injection.
In the present invention, the anti-tumor drug is preferably capsule, more preferably hard capsule, soft capsule or enteric glue Capsule.
In the present invention, the pharmaceutically acceptable carrier and diluent independently preferably include filler, adhesive, One or more of disintegrating agent, lubricant, surfactant and corrigent.
In the present invention, the filler is preferably starch, sucrose, lactose, mannitol, sorbierite, xylitol, crystallite fibre Dimension element or glucose；Described adhesive is preferably cellulose derivative, alginates, gelatin or polyvinylpyrrolidone；It is described to collapse Solving agent is preferably microcrystalline cellulose, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, croscarmellose sodium or crosslinking Povidone；The lubricant is preferably stearic acid, polyethylene glycol, calcium carbonate, sodium bicarbonate, silica, talcum powder or tristearin Sour magnesium；The surfactant is preferably neopelex, stearic acid, Pluronic F68, fat Sour sorb is smooth or polysorbate (tween)；The corrigent is preferably Aspartame, Sucralose or saccharin sodium.
Below with reference to embodiment to the mixture of total tannin in a kind of cymose buckwheat rhizome provided by the invention and epicatechin and its Extracting method and application are described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
1, extracting method: taking cymose buckwheat rhizome 14430g, is ground into the particle of partial size 2mm, is heated with the ethyl alcohol that concentration is 95% Refluxing extraction four times, Extraction solvent quality is respectively the 4 of cymose buckwheat rhizome granular mass, 4,3,2 times, extraction time is followed successively by 60,30, 30,10 minutes, combined extract, filtration, it was 1.06 (55 DEG C) that filtrate, which is concentrated under reduced pressure into relative density in 60 DEG C or less,；Add medicinal extract 10 times of hot water (temperature is 60 DEG C) is measured, is suspended, stands overnight；Supernatant after filtering, with macroporous absorbent resin (D101) column layer Analysis separation, adsorption flow rate 200L/h；First be eluted with water it is colourless to efflux, after with 80% ethanol elution to eluent and trichlorine Until change iron test solution is reactionless, 80% ethanol eluate is collected, it is 1.02 (55 DEG C) that 60 DEG C or less, which are concentrated under reduced pressure into relative density, Spray drying (inlet air temperature is 160 DEG C, and leaving air temp is 70 DEG C, time 6h), obtains Rhizoma Fagopyri Dibotryis extract 1156g.
2, appearance: taking extract to visually observe in the sunlight,
Evaluation: this product is brownish red amorphous powder, and quality is loosely fine and smooth；
3, moisture: taking this product about 0.5g, according to aquametry (Chinese Pharmacopoeia four 0832 determinations of moisture of general rule of version in 2015 The second method of method (oven drying method)) measurement, 9.0% must not be crossed.
Measure moisture: 2%.
4, hygroscopicity: by medicinal powder be packed into dry to constant weight and weigh (m) flat weighing bottle in, thickness is about 2mm, standard Really weigh (mo), it is open in climatic chamber, adjusting temperature is 25 DEG C, and relative humidity 75% is placed 110 hours, not With period weighing (mx), and Moisture percentage is calculated according to following formula.It the results are shown in Table 1:
1 embodiment of table, 1 Rhizoma Fagopyri Dibotryis extract Moisture percentage table
Standing time/h Moisture percentage/%
10 10.12
14 10.23
60 10.08
100 10.25
As the result is shown: Rhizoma Fagopyri Dibotryis extract hygroscopicity variation provided in this embodiment less, illustrates the extract hygroscopicity Low, to being made, the stability after finished product is advantageous.
5, absorbance takes this product 20mg (in terms of dry product), accurately weighed, sets in 100mL measuring bottle, EtOH Sonicate is added to handle (power 150W, frequency 25kHz) makes to dissolve for 30 minutes, lets cool to room temperature, ethyl alcohol is added to be diluted to scale, shake up, use dry filter paper Filtration discards primary filtrate, and precision measures subsequent filtrate 5mL, sets in 50mL measuring bottle, ethyl alcohol is added to be diluted to scale, shake up, according to light splitting light Degree method (four 0401 UV-VIS spectrophotometries of general rule of Chinese Pharmacopoeia version in 2015) measurement, measures at 282nm wavelength and inhales Luminosity must not be lower than 0.30.
Measure absorbance are as follows: 0.32.
6, content assaying method and result:
1) total tannin:
1. this product about 0.25g is taken, it is accurately weighed, it sets in 250mL conical flask, methanol 10mL is added to dissolve it sufficiently, then plus Deionized water 190mL, shakes up, and sets in 35 ± 2 DEG C of water-bath and warms 30 minutes；
2. precision measures the zinc acetate solution 10mL that concentration is 1mol/L, sets in 250mL measuring bottle, adds ammonium hydroxide 7mL, shake up, Dissolve white precipitate；
3. by step 1. in solution slowly injection step 2. in measuring bottle in, and constantly shake, deionized water added to dilute To scale, continue shaking 1 minute, sets and continue warm in 35 ± 2 DEG C of water-bath 30 minutes (interval shaking is for several times), take out, let cool It to room temperature, shakes up, filters, discard primary filtrate, precision measures subsequent filtrate 10mL, sets in 250mL conical flask, add deionized water 150mL, ammonia-ammonium chloride buffer 12.5mL that pH value is 10.0, adds chromium black T indicator 0.1g, shakes up；With 0.025mol/L's Calcium Disodium Versenate titrating solution is titrated to solution and is changed into blue, as terminal, test result blank reality by aubergine Test correction.Every 1mL Calcium Disodium Versenate titrating solution (0.025mol/L) is equivalent to 3.89mg total tannin.
This product is calculated by dry product, must not be less than 60% containing total tannin.
2) epicatechin shines high performance liquid chromatography (Chinese Pharmacopoeia four 0512 high performance liquid chromatography of general rule of version in 2015 Method) measurement
1. chromatographic condition and system suitability are using octadecylsilane chemically bonded silica as filler；With acetonitrile-water (1: It 9) is, mobile phase with phosphorus acid for adjusting pH value 3.00 ± 0.02 (can further adjust when necessary)；Detection wavelength is 282nm, theoretical Plate number is calculated by epicatechin peak should be not less than 3000.
2. the preparation of reference substance solution: precision weighs epicatechin reference substance 10mg, sets in 250mL measuring bottle, adds mobile phase About 20mL, ultrasonic treatment (power 150w, frequency 25kHz) make it dissolve for 10 minutes, take out, anti-cold, are diluted to quarter with mobile phase Degree, shakes up；Precision measures 5mL, sets in 25mL measuring bottle, is diluted to scale with mobile phase, shakes up to get (catechu containing table in every 1mL 80 μ g of element)；
3. the preparation of test solution: this product about 0.25g is taken, it is accurately weighed, add water 30mL, be ultrasonically treated (power 150w, Frequency 25kHz) 30 minutes, it takes out, is transferred in separatory funnel, the chloroform shaking being saturated with water extracts 3 times, every time 30mL discards chloroform liquid, and aqueous is shaken with ethyl acetate and extracted 5 times, each 30mL, and combined ethyl acetate liquid adds anhydrous Appropriate calcium chloride shakes, and filtration, filtrate volatilizes, and residue adds methanol to make it dissolve in right amount, and is quantitatively transferred in 10mL measuring bottle, Add methanol to shake up to scale, filtered with (0.45 μm) of miillpore filter, take subsequent filtrate to get.
4. measuring method: accurate absorption 10 μ L of reference substance and test sample 5-10 μ L respectively, injection liquid chromatograph, measurement, To obtain the final product.
This product (C containing epicatechin15H14O6) 0.40% must not be less than.
As a result: total tannin 85%；Measure epicatechin are as follows: 0.8%.
Embodiment 2
1, extracting method: taking cymose buckwheat rhizome 14430g, is ground into the particle of partial size 3mm, is heated with the ethyl alcohol that concentration is 93% Refluxing extraction four times, Extraction solvent quality is respectively the 4 of cymose buckwheat rhizome granular mass, 4,3,1 times, extraction time is followed successively by 60,30, 30,10 minutes, combined extract, filtration, it was 1.09 (55 DEG C) that filtrate, which is concentrated under reduced pressure into relative density in 60 DEG C or less,；Add medicinal extract 20 times of hot water (temperature is 80 DEG C) is measured, is suspended, stands overnight；Supernatant after filtering, with macroporous absorbent resin (AB-8) column layer Analysis separation, adsorption flow rate 400L/h；First be eluted with water it is colourless to efflux, after with 80% ethanol elution to eluent and trichlorine Until change iron test solution is reactionless, 80% ethanol eluate is collected, it is 1.04 (55 DEG C) that 60 DEG C or less, which are concentrated under reduced pressure into relative density, Spray drying (inlet air temperature is 200 DEG C, and leaving air temp is 100 DEG C, time 8h), obtains Rhizoma Fagopyri Dibotryis extract 1350g.
2, ocular estimate: method is shown in that embodiment 1, this product are brownish red amorphous powder, and quality is loosely fine and smooth；
3, moisture: 5.0%
4, draw moist: detection method the results are shown in Table 2 with embodiment 1:
2 embodiment of table, 2 Rhizoma Fagopyri Dibotryis extract Moisture percentage table
Standing time/h Moisture percentage/%
10 9.45
14 9.24
60 9.51
100 9.37
As the result is shown: Rhizoma Fagopyri Dibotryis extract hygroscopicity variation provided in this embodiment less, illustrates the extract hygroscopicity Low, to being made, the stability after finished product is advantageous.
5, absorbance: 0.34.
6, assay: content assaying method is shown in embodiment 1, as a result are as follows:
1) total tannin: 84.7%；
2) epicatechin: 0.78%.
Comparative example
Chinese patent application CN201110369468.4 disclosed embodiment 1
Rhizoma Fagopyri Dibotryis extract
1, extracting method: taking cymose buckwheat rhizome 14430g, the particle that partial size is less than or equal to 5mm is ground into, with concentration for 95% Ethyl alcohol heating and refluxing extraction four times, Extraction solvent quality is respectively the 6 of cymose buckwheat rhizome granular mass, 4,3,2 times, extraction time according to Secondary is 90,60,60,30 minutes, combined extract, filtration, and it is 1.08 (55 that filtrate, which is concentrated under reduced pressure into relative density in 60 DEG C or less, ℃)；Add 20 times of water of medicinal extract amount, is suspended, stands overnight；Supernatant after filtering, is separated with macroporous adsorbent resin column chromatography；First use Water elution is colourless to efflux, until reactionless with 80% ethanol elution to eluent and ferric trichloride test solution, collects 80% Ethanol eluate, it is 1.08 (55 DEG C) that 60 DEG C or less, which are concentrated under reduced pressure into relative density, and spray drying obtains Rhizoma Fagopyri Dibotryis extract 1056g。
2, moisture: 5.0%.
3, draw moist: detection method the results are shown in Table 3 with embodiment 1.
3 comparative example Rhizoma Fagopyri Dibotryis extract Moisture percentage table of table
Standing time/h Moisture percentage/%
10 12.64
12 12.57
14 12.57
34 12.64
4, absorbance: 0.35.
5, assay: content assaying method is shown in embodiment 1, as a result are as follows:
1) total tannin: 81.57%；
2) epicatechin: 0.75%.
As the result is shown: Rhizoma Fagopyri Dibotryis extract provided in this embodiment is compared with the Rhizoma Fagopyri Dibotryis extract that comparative example provides, surely Qualitative higher, Moisture percentage is smaller, and absorbance is higher, and the content of total tannin and epicatechin increases.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (10)

1. the extracting method of the mixture of total tannin and epicatechin in a kind of cymose buckwheat rhizome, which comprises the following steps:
Cymose buckwheat rhizome is crushed to 2~3mm of partial size, obtains cymose buckwheat rhizome particle；
The cymose buckwheat rhizome particle is extracted with alcohol reflux, obtains extracting solution；
It is 1.06~1.09 that gained filtrate decompression after extracting solution filtering, which is concentrated into relative density, obtains medicinal extract；
Gained supernatant after filtering, is separated with macroporous adsorbent resin column chromatography, first uses water after the medicinal extract is mixed with hot water It is colourless to be eluted to efflux, then with 80% ethanol elution to efflux and ferric trichloride test solution it is reactionless until, regather 80% Ethyl alcohol efflux, obtains eluent, and the temperature of the hot water is 60~80 DEG C；
It is 1.02~1.04 that the eluent, which is concentrated into relative density, is spray-dried to get total tannin in cymose buckwheat rhizome and table The mixture of theine.
2. extracting method according to claim 1, which is characterized in that the number that the alcohol reflux extracts is 4 times, described The mass ratio of ethyl alcohol and cymose buckwheat rhizome particle is respectively 4:1,4:1,3:1 and 1~2:1, the alcohol reflux when alcohol reflux extracts The time of extraction is followed successively by 60,30,30 and 10min.
3. extracting method according to claim 1, which is characterized in that the volume ratio of the medicinal extract and hot water be 1:10~ 20。
4. extracting method according to claim 1, which is characterized in that the macroporous absorbent resin is D101 or AB-8.
5. extracting method according to claim 1 or 4, which is characterized in that the partial size of the macroporous absorbent resin be 0.3~ 1.25mm, specific surface area are 600~700m2/ g, average pore size are 8.5~9.5nm.
6. extracting method according to claim 1 or 4, which is characterized in that the adsorption flow rate of the macroporous absorbent resin is 200~400L/h.
7. extracting method according to claim 1, which is characterized in that the inlet air temperature of the spray drying be 160 DEG C~ 200 DEG C, leaving air temp is 70 DEG C~100 DEG C, and the time of the spray drying is 6~8h.
8. total tannin that the described in any item extracting methods of claim 1~7 are extracted from cymose buckwheat rhizome and epicatechin Mixture.
9. the mixture of the total tannin according to any one of claims 8 extracted from cymose buckwheat rhizome and epicatechin prepare it is antitumor Application in drug.
10. application according to claim 9, which is characterized in that the anti-tumor drug includes extracting from cymose buckwheat rhizome Mixture, pharmaceutically acceptable carrier and the diluent of the total tannin and epicatechin that arrive.
CN201910113968.8A 2019-02-14 2019-02-14 The mixture and its extracting method of total tannin and epicatechin and application in a kind of cymose buckwheat rhizome Withdrawn CN109620864A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112022906A (en) * 2020-08-28 2020-12-04 吉林农业大学 Preparation method of buckwheat husk non-flavone substance

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112022906A (en) * 2020-08-28 2020-12-04 吉林农业大学 Preparation method of buckwheat husk non-flavone substance
CN112022906B (en) * 2020-08-28 2022-02-15 吉林农业大学 Preparation method of buckwheat husk non-flavone substance

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Application publication date: 20190416