CN108339086A - A kind of preparation method of Turmeric P.E - Google Patents
A kind of preparation method of Turmeric P.E Download PDFInfo
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- CN108339086A CN108339086A CN201710051021.XA CN201710051021A CN108339086A CN 108339086 A CN108339086 A CN 108339086A CN 201710051021 A CN201710051021 A CN 201710051021A CN 108339086 A CN108339086 A CN 108339086A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/12—Ketones
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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)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/906—Zingiberaceae (Ginger family)
- A61K36/9066—Curcuma, e.g. common turmeric, East Indian arrowroot or mango ginger
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- 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
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
-
- 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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- 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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- 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
Abstract
The present invention provides a kind of preparation method of Turmeric P.E, this method is using turmeric medicinal material as raw material, and by crushing, alcohol extracting, concentration extracts, and crystallizes, washing, dry and preparation Turmeric P.E.Product colour is gorgeous, (the C containing curcumin wherein in Turmeric P.E21H20O6), Demethoxycurcumin (C20H18O5) and Bisdemethoxycurcumin (C19H16O4) total amount be 45.0% 70.0%, the and (C containing curcumin21H20O6), Demethoxycurcumin (C20H18O5) and Bisdemethoxycurcumin (C19H16O4) total amount be more than curcumin chemical compounds 93.0%.Containing curcumin (C21H20O6) it is 40.0% 60.0%.The product complies fully with the requirement that feeds intake of reducing lipid and dredging collaterals soft capsule.This method is extracted using a step, and two step alcohol deposition methods ensure that the quality of Turmeric P.E, and technological operation is simple, deoils with obvious effects, is conducive to product drying, and process stabilizing, is suitble to industrialized production.
Description
Technical field
The present invention relates to a kind of preparation methods of Turmeric P.E, belong to active ingredient of natural plant extraction and separation technology neck
Domain.
Background technology
Turmeric is the dry rhizome of Zingiber curcuma Curcuma longa L., is herbaceos perennial, is《In
State's pharmacopeia》The conventional Chinese medicine of collection；Its bitter is warm-natured, returns spleen, Liver Channel, there is blood-breaking, inducing meastruation to relieve menalgia effect.It is mainly lived
Property ingredient be curcumin chemical compounds, including three kinds of active constituents, respectively curcumin, double remove methoxy at Demethoxycurcumin
Base curcumin.
Modern medicine study show curcumin have anti-oxidant, anti-inflammatory, lipid-loweringing, liver protection, antitumor, antifertility, antidepression,
Prevent senile dementia and other effects, curcumin is also widely used food additives both at home and abroad, therefore curcumin is a kind of day
So, green, dietotherapeutic functional health care food, is widely used in the fields such as medicine, health products, food, cosmetics.
Curcumin is mainly produced from the rhizome of zingiberaceous plant turmeric, is carried using the various extractions that can dissolve curcumin
It takes, recycling design obtains curcumin crude product, to obtain high-purity curcumin, it is necessary to initial gross separation purifying is carried out to curcumin crude product,
And difficult point is how to remove oil substances and turmeric resinous matter similar with curcumin polarity.
It is the technique generally used both at home and abroad at present to extract curcumin from turmeric with organic solvent (such as ethyl alcohol).However it uses
The turmeric paste that this method is extracted is the mixture of the impurity such as curcumin and lipid, and this product pigment content is low, root
Difficulty reaches the quality index of total pigment content >=90% of FAO/WHO standards requirement, and is difficult to drying, is unfavorable for packaging, fortune
Defeated and use.
In the preparation patent of Turmeric P.E extraction part mainly using organic solvent in addition there are sour water -ol and buck into
Row extraction, patent CN200710304013.8 extract curcumin chemical compounds using buck, and method saves organic solvent usage amount.
Active ingredient is more than 90% in Turmeric P.E；Patent CN200910074614.3 obtains curcuma oil using alcohol-sour water extraction method
Resin is adsorbed using dedicated adsorbent, and desorption obtains the Turmeric P.E of high-purity；Patent
CN201310088988.7 obtains extracting solution, acid adding precipitation using the method for buck extraction, and the method for the molten purifying of alcohol obtains turmeric
Extract；Patent CN201310124957.2 extracts object, macroporous resin adsorption ethanol gradient elution using alcohol-amino acid water
It is purified to obtain Turmeric P.E；Patent CN201310531265.X uses buck extract, then uses petroleum ether extraction ginger
Butter, then precipitated with sour water, alcohol dissolved crystalline substance purifies to obtain Turmeric P.E；In addition to said extracted method also has patent
CN200810032183.X has carried out means of supercritical extraction to the curcuma oil in turmeric, and this method is to be extracted to turmeric constituents
Research；Patent CN201110253477.7 carries out the preparation of Turmeric P.E using dynamic countercurrent extractive technique, and method is novel, obtains
The Turmeric P.E purity arrived is high, but equipment investment is big；In the purification part of Turmeric P.E, patent CN201510658394.4
Using the inclusion technique of beta cyclodextrin, 3 kinds of active constituents in Turmeric P.E crude product are detached；Patent
CN88105879.3, to the difference of the solubility of curcumin and curcuma oil and rcumenol, is realized to curcumin using different solvents
The single step of class compound, curcuma oil and rcumenol produces, and obtains curcumin chemical compounds；In patent CN200710051789.3
Medicinal extract after being concentrated to extraction using adsorbent is carried out de-oiling using the solvent of opposed polarity after adsorbing and elutes curcumin
Class compound obtains the higher Turmeric P.E of purity；Patent CN200810080239.9 is extracted using alcohol and alkanes
It obtains carrying out separation curcuma oil using saliferous release agent after extracting solution concentrates, reduces the usage amount of nonpolar solvent, subsequently adopt
Purifying curcumin is carried out with resin adsorption, obtained turmeric cellulose content is higher；Patent CN200910114423.5 is carried using turmeric
It is raw material to take object crude product, is removed to the impurity in extract using mixed solvent, high-purity is obtained using alcohol crystal
Turmeric P.E；Patent CN201010103128.2 using ether extraction remove volatile oil, cation exchange resin, film concentration and
Alumina column chromatography isolates and purifies, and recrystallizing methanol obtains the Turmeric P.E of high-purity；Patent CN201010103117.4 is adopted
After petroleum ether degreasing, sodium salicylate alcoholic solution extraction, macroporous absorption purifies to obtain the Turmeric P.E of high-purity；Patent
CN201610023830 uses liquid-liquid extraction, alcohol-water to crystallize twice, will inhibit the de-methoxy of cancer cell hyperplasia in turmeric
Curcumin, the Bisdemethoxycurcumin for preventing cell lipid peroxide from being formed remove, and have had to the curcumin of high-purity.
In conclusion above-mentioned patent all realizes the preparation and purification process of Turmeric P.E, wherein extraction part is organic
The extraction of solvent is small to the destruction of active ingredient in Turmeric P.E, and extraction is abundant, with the obvious advantage compared with other extracting modes, but takes
With higher.Purification part is purified using adsorbent, and obtained purity is higher, but uses macroreticular resin and other absorption
Agent has a certain impact to product quality, and the production cycle is longer.Crystallization processes are advantageous compared with adsorption and purification.But it is all
Patent is to highlight the extraction purification of curcumin, does not pay close attention to anticancer, the significantly more de-methoxy turmeric of antioxidation
Element, Bisdemethoxycurcumin, Turmeric P.E prepared by this patent include curcumin, Demethoxycurcumin and double remove methoxy
Base curcumin, and the ratio between three complies fully with requirement of the reducing lipid and dredging collaterals soft capsule to Turmeric P.E, reducing lipid and dredging collaterals
It is optimal proportion that Turmeric P.E component ratio in soft capsule, which passes through experimental verification,.
Invention content
In view of this, the main purpose of the present invention is to provide a kind of uses that feeds intake complying fully with reducing lipid and dredging collaterals soft capsule
It is required that the preparation method of curcumin extraction.
To achieve the goals above, the present invention provides the following technical solutions：
A kind of preparation method of Turmeric P.E, includes the following steps：
(a) 50%-95% low-alcohol solutions or acetone is used to extract turmeric medicinal material with n-hexane mixed solution, wherein described low
The volume of grade alcoholic solution or acetone and n-hexane mixed solution is that 6-20 times of turmeric medicinal material weight is measured, and extraction time is that 1-4 is small
When, Extracting temperature is 45 DEG C -80 DEG C, and extraction time is 2-4 times；
(b) extracting solution weight obtained by step (a) is concentrated into 0.1-1 times of medicinal material weight, concentrate weight 0.1- is added
The low-alcohol solution of 0.4 times of volume, refrigeration staticly settle 12-24 hours, remove insoluble matter；
(c) petroleum ether of 1-2 times of volume of liquid weight is added into liquid obtained by step (b), it is quiet after stirring 10-30 minutes
It sets 12-24 hours, extracts upper layer petroleum ether layer, concentration and recovery petroleum ether obtains by-product curcuma oil；
(d) lower liquid weight obtained by step (c) is concentrated into 0.05~0.2 times of medicinal material weight, concentrate weight is added
80%~95% low-alcohol solution of 0.3~0.5 times of volume of amount, stands 12-24h after stirring evenly, centrifuge, and collects crystallization；
(e) it will be crystallized obtained by step (d), washed with corresponding 80%~95% low-alcohol solution, centrifuged again, obtained
To crystallization；
(f) low temperature drying being crystallized obtained by step (e), being crushed, sieving obtains Turmeric P.E.
Preferably, in the step (a), (b) and (d) lower alcohol be selected from methanol, ethyl alcohol, propyl alcohol, butanol, amylalcohol or oneself
Alcohol, preferred alcohol.
Preferably, the volume ratio of low-alcohol solution or acetone and n-hexane mixed solution is 2 in the step (a):1~1:
2。
Preferably, 50%-95% low-alcohol solutions described in step (a) is selected from 50% ethanol solution, 70% ethanol solution
Or 95% ethanol solution；It is 2 that the acetone, which is selected from acetone and n-hexane volume ratio with n-hexane mixed solution,:1, acetone with just
The volume ratio of hexane is 1:1 or the volume ratio of acetone and n-hexane be 1:2.
Preferably, the volume of the low-alcohol solution described in step (a) or acetone and n-hexane mixed solution is medicinal material
8~16 times of weight, extraction time are 1.5-3 hours, and Extracting temperature is 50 DEG C -60 DEG C, and extraction time is 2-3 times.
Preferably, extracting solution described in step (b) is concentrated into 0.1~0.2 times of medicinal material weight, adds concentrate weight
The low-alcohol solution of 0.25 times of amount of amount.
Preferably, lower liquid weight described in step (d) is concentrated into 0.05~0.2 times of medicinal material weight, and preferably 0.1
Times, 80%~95% low-alcohol solution of 0.4 times of amount of concentrate weight is added.
Preferably, drying temperature≤50 DEG C of step (f) low temperature drying, drying mode are selected from vacuum drying, spraying
Drying, microwave drying, freeze-drying or constant pressure and dry.
The preparation method of the Turmeric P.E of the present invention is proposed or is mixed extraction by organic solvent list and obtains turmeric oleoresin,
It is extracted using petroleum ether, carries out crystallization experiment using the ethyl alcohol of various concentration, obtain that there is (the C containing curcumin21H20O6), go
Methoxyl group curcumin (C20H18O5) and Bisdemethoxycurcumin (C19H16O4) total amount be 45.0%-70.0%, and contain turmeric
Element (C21H20O6), Demethoxycurcumin (C20H18O5) and Bisdemethoxycurcumin (C19H16O4) total amount should be greater than turmeric
The 93.0% of chlorins compound.Containing curcumin (C21H20O6) be 40.0%-60.0% feature Turmeric P.E.
The innovation of the invention consists in that establishing the satisfactory Turmeric P.E that different ethanol concentration crystallizes, surpass
Go out concentration of alcohol and is unable to get the Turmeric P.E raw material for meeting and preparing reducing lipid and dredging collaterals soft capsule.In addition, changing different concentrations
The solvent of volume and crystallization can obtain the higher Turmeric P.E of purity, but be not suitable for reducing lipid and dredging collaterals soft capsule preparation
Preparation demand.
The method using alcohol crystal of the present invention carries out preparing Turmeric P.E, and turmeric class is realized in crystallisation step
The separation for closing object and turmeric oily substance, it is dry fundamentally to solve the problems, such as that Turmeric P.E is difficult to.
The preparation method of the Turmeric P.E of the present invention is simple, easy to operate with technical process, is adsorbed without using other
Agent, it is comparatively safe it is reliable, the requirement to equipment is relatively low, conducive to shop worker's operation, product stable quality the features such as.Its
Product has the (C containing curcumin21H20O6), Demethoxycurcumin (C20H18O5) and Bisdemethoxycurcumin (C19H16O4)
Total amount is 45.0%-70.0%, and (the C containing curcumin21H20O6), Demethoxycurcumin (C20H18O5) and double de-methoxy ginger
Flavine (C19H16O4) total amount should be greater than the 93.0% of curcumin chemical compounds.Containing curcumin (C21H20O6) it is 40.0%-
60.0%.And meet the feature used that feeds intake of reducing lipid and dredging collaterals soft capsule.
Specific embodiment
Following is that the present invention is further explained in conjunction with specific embodiments.But these embodiments be only limitted to illustrate the present invention without
It is for limiting the scope of the invention.
Embodiment 1
Turmeric medicinal material powder 1kg is weighed, is put into extraction flask, 50% ethyl alcohol of 5 times of amounts is added, twice in 55 DEG C of extractions, point
Indescribably take 2 hours and 1.5 hours.After extraction, upper layer extracting solution is extracted, after merging extracting solution, filtrate, vacuum is obtained by filtration
Be concentrated into medicinal material weight 0.1 times goes out cream.The ethyl alcohol of about 0.25 times of amount of cream weight is added into cream, stirs to dissolving
Afterwards, refrigeration stands 24 hours, and removal bucket bottom insoluble matter is weighed.Petroleum ether (the 60-90 of cream weight isometric (g/ml) is added
DEG C), it stirs evenly, timing is stirred 30 minutes, is stood for 24 hours.Upper layer petroleum ether layer is extracted, is discarded.Lower layer's extract liquor vacuum is dense
Be reduced to medicinal material weight 0.05 times goes out cream.80% ethyl alcohol of 0.4 times of amount (g/g) of cream weight is added, stirs evenly, refrigeration is stood
12h.Supernatant liquid is extracted, is discarded, lower sediment stirs evenly, centrifugation.The precipitation after centrifugation is taken to be added the 80% of equivalent (g/g)
Ethyl alcohol stirs evenly, centrifugation, and the 80% ethanol rinse crystallization of identical times of amount is used in combination.Finished product 30.5g is obtained after dry, pulverize.Content
It measures, result is containing curcumin (C21H20O6), Demethoxycurcumin (C20H18O5) and Bisdemethoxycurcumin (C19H16O4)
Total amount be 60.2%, the and (C containing curcumin21H20O6), Demethoxycurcumin (C20H18O5) and Bisdemethoxycurcumin
(C19H16O4) total amount should be greater than the 96.4% of curcumin chemical compounds.Containing curcumin (C21H20O6) it is 57.2%
Embodiment 2
Turmeric medicinal material powder 1kg is weighed, is put into extraction flask, 70% ethyl alcohol of 8 times of amounts is added, twice in 60 DEG C of extractions, point
Indescribably take 3 hours and 2 hours.After extraction, upper layer extracting solution is extracted, after merging extracting solution, filtrate is obtained by filtration, vacuum is dense
Be reduced to medicinal material weight 0.14 times goes out cream.The ethyl alcohol of about 0.25 times of amount of cream weight is added into cream, stirs to dissolving
Afterwards, refrigeration stands 18 hours, and removal bucket bottom insoluble matter is weighed.Petroleum ether (the 60-90 of cream 1.5 times of volumes (g/ml) of weight is added
DEG C), it stirs evenly, timing is stirred 10 minutes, is stood for 24 hours.Upper layer petroleum ether layer is extracted, is discarded.Lower layer's extract liquor vacuum is dense
Be reduced to medicinal material weight 0.1 times goes out cream.90% ethyl alcohol of 0.4 times of amount (g/g) of cream weight is added, stirs evenly, refrigeration is stood
24h.Supernatant liquid is extracted, is discarded, lower sediment stirs evenly, centrifugation.The precipitation after centrifugation is taken to be added the 90% of equivalent (g/g)
Ethyl alcohol centrifuges again after stirring evenly, and the 90% ethanol rinse crystallization of identical times of amount is used in combination.Finished product is obtained after dry, pulverize
29.5g.Assay, result are containing curcumin (C21H20O6), Demethoxycurcumin (C20H18O5) and double de-methoxy turmerics
Element (C19H16O4) total amount be 66.2%, the and (C containing curcumin21H20O6), Demethoxycurcumin (C20H18O5) and double remove methoxy
Base curcumin (C19H16O4) total amount should be greater than the 98.1% of curcumin chemical compounds.Containing curcumin (C21H20O6) it is 58.5%
Embodiment 3
Turmeric medicinal material powder 1kg is weighed, is put into extraction flask, 95% ethyl alcohol of 6 times of amounts is added, three times in 50 DEG C of extractions, point
It indescribably takes 3 hours, 2 hours and 1.5 hours.After extraction, upper layer extracting solution is extracted, after merging extracting solution, filter is obtained by filtration
Liquid, be concentrated in vacuo to medicinal material weight 0.2 times go out cream.The ethyl alcohol of about 0.25 times of amount of cream weight is added into cream, is sufficiently stirred
Even refrigeration stands 12 hours to after dissolving, and removal bucket bottom insoluble matter is weighed.The petroleum ether of cream 2 times of volumes (g/ml) of weight is added
(60-90 DEG C), stirs evenly, and timing is stirred 20 minutes, stands for 24 hours.Upper layer petroleum ether layer is extracted, is discarded.By lower layer's extract liquor
It is concentrated in vacuo into 0.1 times of medicinal material weight and goes out cream.95% ethyl alcohol of 0.4 times of amount (g/g) of cream weight is added, stirs evenly,
Refrigeration stands 12h.Quiet supernatant liquid is extracted, is discarded, lower sediment stirs evenly, centrifugation.Take the precipitation after centrifugation that equivalent is added
(g/g) 95% ethyl alcohol, centrifuges again after stirring evenly, and the 95% ethanol rinse crystallization of identical times of amount is used in combination.After dry, pulverize
Obtain finished product 28.7g.Assay, result are containing curcumin (C21H20O6), Demethoxycurcumin (C20H18O5) and double remove methoxy
Base curcumin (C19H16O4) total amount be 69.1%, the and (C containing curcumin21H20O6), Demethoxycurcumin (C20H18O5) and it is double
Demethoxycurcumin (C19H16O4) total amount should be greater than the 97.8% of curcumin chemical compounds.Containing curcumin (C21H20O6) be
59.7%.
Embodiment 4
Turmeric medicinal material powder 1kg is weighed, is put into extraction flask, the acetone and n-hexane mixed solution (2 of 4 times of amounts is added:1),
Twice in 55 DEG C of extractions, it extracts 2 hours and 2 hours respectively.After extraction, upper layer extracting solution is extracted, after merging extracting solution, mistake
Filter obtains filtrate, and be concentrated in vacuo to medicinal material weight 0.125 times goes out cream.The ethyl alcohol of about 0.25 times of amount of cream weight is added into cream,
It stirs to dissolving, refrigeration stands 24 hours, and removal bucket bottom insoluble matter is weighed.2 times of volume (g/ of cream weight are added
Ml petroleum ether (60-90 DEG C)), stirs evenly, and timing is stirred 20 minutes, stands 12h.Upper layer petroleum ether layer is extracted, is discarded.It will
Lower layer's extract liquor be concentrated in vacuo to medicinal material weight 0.1 times goes out cream.85% ethyl alcohol of 0.4 times of amount (g/g) of cream weight is added, stirs
It mixes uniformly, refrigeration stands 12h.Supernatant liquid is extracted, is discarded, lower sediment centrifuges after stirring evenly.The precipitation after centrifugation is taken to add
85% ethyl alcohol for entering equivalent (w/w), centrifuges again after stirring evenly, and the 85% ethanol rinse crystallization of identical times of amount is used in combination.It is dry,
Finished product 31.2g is obtained after crushing.Assay, result are containing curcumin (C21H20O6), Demethoxycurcumin (C20H18O5) and it is double
Demethoxycurcumin (C19H16O4) total amount be 65.7%, the and (C containing curcumin21H20O6), Demethoxycurcumin
(C20H18O5) and Bisdemethoxycurcumin (C19H16O4) total amount should be greater than the 96.5% of curcumin chemical compounds.Containing turmeric
Element (C21H20O6) it is 57.4%
Embodiment 5
Turmeric medicinal material powder 1kg is weighed, is put into extraction flask, the acetone and n-hexane mixed solution (1 of 6 times of amounts is added:1),
Twice in 50 DEG C of extractions, it extracts 2 hours and 2 hours respectively.After extraction, upper layer extracting solution is extracted, after merging extracting solution, mistake
Filter obtains filtrate, and be concentrated in vacuo to medicinal material weight 0.15 times goes out cream.The ethyl alcohol of about 0.25 times of amount of cream weight is added into cream, fills
Divide after being evenly stirred until dissolving, refrigeration stands 12 hours, and removal bucket bottom insoluble matter is weighed.It is isometric (g/ml) that cream weight is added
Petroleum ether (60-90 DEG C), stir evenly, timing stir 10 minutes, stand for 24 hours.Upper layer petroleum ether layer is extracted, is discarded.Will under
Layer extract liquor is concentrated in vacuo to 0.1 times of medicinal material weight and goes out cream.95% ethyl alcohol of 0.4 times of amount (w/w) of cream weight, stirring is added
Uniformly, refrigeration is stood for 24 hours.Supernatant liquid is extracted, is discarded, lower sediment centrifuges after stirring evenly.The precipitation after centrifugation is taken to be added
95% ethyl alcohol of equivalent (g/g), centrifuges again after stirring evenly, and the 95% ethanol rinse crystallization of identical times of amount is used in combination.It is dry, powder
Finished product 25.6g is obtained after broken.Assay, result are containing curcumin (C21H20O6), Demethoxycurcumin (C20H18O5) and double go
Methoxyl group curcumin (C19H16O4) total amount be 64.8%, the and (C containing curcumin21H20O6), Demethoxycurcumin (C20H18O5)
With Bisdemethoxycurcumin (C19H16O4) total amount should be greater than the 96.2% of curcumin chemical compounds.Containing curcumin
(C21H20O6) it is 57.1%
Embodiment 6
Turmeric medicinal material powder 1kg is weighed, is put into extraction flask, the acetone and n-hexane mixed solution (1 of 4 times of amounts is added:2),
Three times in 60 DEG C of extractions, it extracts 2 hours, 2 hours and 1.5 hours respectively.After extraction, upper layer extracting solution is extracted, merging carries
After taking liquid, filtrate is obtained by filtration, be concentrated in vacuo to medicinal material weight 0.18 times goes out cream.About 0.25 times of amount of cream weight is added into cream
Ethyl alcohol, stir to dissolving, refrigeration stands 24 hours, and removal bucket bottom insoluble matter is weighed.Cream weight 1.5 is added
The petroleum ether (60-90 DEG C) of times volume (g/ml), stirs evenly, and timing is stirred 30 minutes, stands 12h.Extract upper layer petroleum ether
Layer, discards.0.05 times that lower layer's extract liquor is concentrated in vacuo to medicinal material weight goes out cream.0.4 times of amount (g/g) of cream weight is added
80% ethyl alcohol, stirs evenly, and refrigeration is stood for 24 hours.Supernatant liquid is extracted, is discarded, lower sediment centrifuges after stirring evenly.Take centrifugation
80% ethyl alcohol of equivalent (g/g) is added in precipitation afterwards, is centrifuged again after stirring evenly, and 80% ethanol rinse of identical times of amount is used in combination
Crystallization.Finished product 24.2g is obtained after dry, pulverize.Assay, result are containing curcumin (C21H20O6), Demethoxycurcumin
(C20H18O5) and Bisdemethoxycurcumin (C19H16O4) total amount be 68.8%, the and (C containing curcumin21H20O6), de-methoxy
Curcumin (C20H18O5) and Bisdemethoxycurcumin (C19H16O4) total amount should be greater than the 99.0% of curcumin chemical compounds.
Containing curcumin (C21H20O6) it is 59.8%
It should be understood that after reading the above teachings of the present invention, those skilled in the art can make the present invention
Various changes or modification, these equivalent forms also fall within the scope of the appended claims of the present application.
Claims (9)
1. a kind of preparation method of Turmeric P.E, which is characterized in that this method includes the following steps：
(a) 50%-95% low-alcohol solutions or acetone is used to extract turmeric medicinal material with n-hexane mixed solution, wherein the lower alcohol
The volume of solution or acetone and n-hexane mixed solution is that 6-20 times of turmeric medicinal material weight is measured, and extraction time is 1-4 hours, is carried
It is 45 DEG C -80 DEG C to take temperature, and extraction time is 2-4 times；
(b) extracting solution weight obtained by step (a) is concentrated into 0.1-1 times of medicinal material weight, 0.1-0.4 times of concentrate weight is added
The low-alcohol solution of volume, refrigeration staticly settle 12-24 hours, remove insoluble matter；
(c) petroleum ether of 1-2 times of volume of liquid weight is added into liquid obtained by step (b), stirring is stood after 10-30 minutes
12-24 hours, upper layer petroleum ether layer is extracted, concentration and recovery petroleum ether obtains by-product curcuma oil；
(d) lower liquid weight obtained by step (c) is concentrated into 0.05~0.2 times of medicinal material weight, concentrate weight is added
80%~95% low-alcohol solution of 0.3~0.5 times of volume stands 12-24h after stirring evenly, crystallization is collected in centrifugation；
(e) it will be crystallized obtained by step (d), washed with corresponding 80%~95% low-alcohol solution, centrifuged again, tied
It is brilliant；
(f) low temperature drying being crystallized obtained by step (e), being crushed, sieving obtains Turmeric P.E.
2. preparation method according to claim 1, which is characterized in that step (a), (b) and lower alcohol described in (d) are selected from
Methanol, ethyl alcohol, propyl alcohol, butanol, amylalcohol or hexanol, preferred alcohol.
3. preparation method according to claim 1, which is characterized in that in the step (a) low-alcohol solution or acetone with
The volume ratio of n-hexane mixed solution is 2:1~1:2.
4. the preparation method of Turmeric P.E according to claim 1, which is characterized in that 50%- described in step (a)
95% low-alcohol solution is selected from 50% ethanol solution, 70% ethanol solution or 95% ethanol solution；The acetone is mixed with n-hexane
It is 2 that conjunction solution, which is selected from acetone and n-hexane volume ratio,:1, the volume ratio of acetone and n-hexane is 1:1 or acetone and n-hexane
Volume ratio be 1:2.
5. the preparation method of Turmeric P.E according to claim 1, which is characterized in that described low described in step (a)
The volume of grade alcoholic solution or acetone and n-hexane mixed solution is 8~16 times of medicinal material weight, and extraction time is 1.5-3 hours,
Extracting temperature is 50 DEG C -60 DEG C, and extraction time is 2-3 times.
6. preparation method according to claim 1, which is characterized in that extracting solution described in step (b) is concentrated into medicinal material
0.1~0.2 times of weight adds the low-alcohol solution of 0.25 times of amount of concentrate weight.
7. wanting preparation method according to claim 1, which is characterized in that lower liquid weight described in step (d) concentrates
To 0.05~0.2 times of medicinal material weight, preferably 0.1 times, 80%~95% lower alcohol that 0.4 times of amount of concentrate weight is added is molten
Liquid.
8. preparation method according to claim 1, which is characterized in that the drying temperature of step (f) low temperature drying≤
50 DEG C, drying mode is selected from vacuum drying, spray drying, microwave drying, freeze-drying or constant pressure and dry.
9. the preparation method of Turmeric P.E according to any one of claims 1-7, which is characterized in that the turmeric
Total amount containing curcumin, Demethoxycurcumin and Bisdemethoxycurcumin in extract is 45.0%-70.0%, and contains ginger
The total amount of flavine, Demethoxycurcumin and Bisdemethoxycurcumin should be greater than the 93.0% of curcumin chemical compounds, contain ginger
Flavine is 40.0%-60.0%.
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