CN106831808B - A kind of technique of the rapid extraction eurycomanone from Tongkat Ali - Google Patents
A kind of technique of the rapid extraction eurycomanone from Tongkat Ali Download PDFInfo
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- CN106831808B CN106831808B CN201710230605.3A CN201710230605A CN106831808B CN 106831808 B CN106831808 B CN 106831808B CN 201710230605 A CN201710230605 A CN 201710230605A CN 106831808 B CN106831808 B CN 106831808B
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- tongkat ali
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/10—Spiro-condensed systems
Abstract
A kind of technique of the rapid extraction eurycomanone from Tongkat Ali, the technique include carrying out subcritical abstraction with ethanol after Tongkat Ali raw material is crushed, concentrated, and spiral shell centrifugation of crouching, obtain centrifuged supernatant；By macroporous resin column in centrifuged supernatant, gradient elution, the eluent concentration plus alcohol crystallization of collection dilute after filtering, add activated carbon decolorizing, filtering, concentration, crystallization, dry eurycomanone product.Using the high purity 98% of eurycomanone obtained by this technique, ultimate yield is more than 90%.The present invention uses the subcritical pure utilization rate for putting forward technology and improve the rate of transform and Tongkat Ali of active principle, reduces production cost, improves production efficiency；In addition this technique simply continuous operation property is strong, is adapted to large-scale industrial production.
Description
Technical field
The invention belongs to effective ingredients in plant extraction to separate, and in particular to one kind is adapted to industrial from Tongkat Ali
The technique of rapid extraction separation of high-concentration eurycomanone.
Background technology
The report printed according to a Straits Times week on May 1, in 999, assistant Harry of Malaysian university not Harmer
Doctor Sha A points out that the male mouse after feeding Tongkat Ali extract solution, sexual behaviour is active, and the number of female mice mating is frequent.Cause
The startling magical effect of Tongkat Ali, therefore extensively bought and eat by visitors such as Japan, the U.S., but also because rare numbers form
For the plant of Malaysian national legislation protection.Mahathir period in place, Tongkat Ali is widelyd popularize, makes Malaysia
The national treasure of West Asia " most young ", Malaysia and the local common people such as Indonesia since ancient times, with regard to normal infusion, its tree root is drunk.
It is said that the plant essence of Tongkat Ali can get well, renew one's youth, however more allow people it is noted that its another good name
" natural philter " or " natural medea ".It is local it also referred to as Pasak Bumi, it is meant that " walking of Ali is turned
Cane（Ali's Walking Stick）", " crutch " is conventional " penis " synonym in Malay, is thus revealed out to man
The influence of scholar's property effect.But it is Yang invigorating medicine that the effect of Tongkat Ali, which runs far deeper than,.Malaysian university's clinical test proves
Its multiple function, its extract also have lifting muscle power and vigor, lessen fatigue, sterilize, antiulcer, antipyretic efficiency, also
Having improves various illness such as hypertension, diabetes and other effects.According to Lianhe Zaobao in 2002, Tongkat Ali was also found to contain
There are some chemical compositions for being capable of anticancer and anti-AIDS.Malaysian forest research institute chief inspector Ah all Lhasa points out, preliminaryization
The chemical composition tested contained by display Tongkat Ali is more more effective than existing cancer therapy drug, particularly anti-uterus cancer drug.In Malaysia
West Asia, Tongkat Ali have the title of Malaysia ginseng, are always taken as postnatal nourishing product, as treatment diabetes, hypertension, prostate
Inflammation, pulmonary tuberculosis, fever, jaundice and dysentery.Quassinoids compound is its main active in Tongkat Ali, eurycomanone (
Eurycomanone, EN) it is wherein most representational.Application in health products, medicine at present is low content or ratio
Product, it is following in order to reach more preferable effect, it is necessary to the eurycomanone of higher amount.
A kind of existing method that eurycomanone is extracted from Tongkat Ali, as CN103408564B discloses Tongkat Ali plant
The extraction and purification process of middle eurycomanone, comprises the following steps:(1) preparation of Tongkat Ali medicinal extract；(2) degreasing of concentrate；
(3) degreaser extracts eurycomanone composition；(4) pillar layer separation；(5) eluent decolourizes；(6) concentrate, crystallization；(7) purify；
(8) filtering, dry eurycomanone product.But its technique extracts the insufficient, production cycle to Tongkat Ali material effective component
It is long, using organic solvent is more, production capacity is small, production cost is high, is not suitable for large-scale production.And for example CN201610743803.5 is disclosed
A kind of industrial production process of the separating high-purity eurycomanone from Tongkat Ali, comprises the following steps:(1) enzyme-added immersion:Will
Tongkat Ali raw material soaking enzyme-added enzymolysis, obtains enzymolysis Tongkat Ali in water；(2) heating extraction:Will enzymolysis Tongkat Ali heating
Extraction, obtains Tongkat Ali leaching liquor；(3) centrifugal degreasing:After cooling, degreasing is centrifuged, obtains degreaser；(4) ultrafiltration, nanofiltration:Will be de-
Fat liquid carries out ultrafiltration, and nanofiltration obtains eurycomanone nanofiltration retentate fluid；(5) resin chromatography:By macropore tree in eurycomanone nanofiltration retentate fluid
Fat, gradient elution, the concentration of target phase eluent is collected, obtains concentrate；(6) alcohol phase crystallization, dry, filtering, crystallization, washing,
Dry, obtain high-purity eurycomanone.But its technique to Tongkat Ali material effective component extract it is insufficient, to Feedstock treating when
Between it is long, and sleeping spiral shell centrifugation is carried out in the program, tubular type centrifugation, ultrafiltration, the solution treating capacity of nanofiltration are all that Tongkat Ali is former
8-12 times of doses so that workload is excessively huge, and equipment investment is big, and production difficulty is big, and production cost is high, is not suitable for scale life
Production.
The content of the invention
It is an object of the invention to overcome prior art exist it is above-mentioned deficiency in the case of, there is provided one kind from Tongkat Ali
The technique of rapid extraction eurycomanone, the technique is simple and quick, low energy consumption, low cost, pollution-free, the eurycomanone high income of acquisition,
Purity is high, is suitable for large-scale production.
To achieve the above object, the technical solution adopted by the present invention is as follows：One kind wide tassel of rapid extraction from Tongkat Ali
The technique of ketone, the processing step are as follows：
（1）Subcritical abstraction：Using Tongkat Ali as raw material, inserted after crushing in subcritical abstraction kettle, be with volume fraction
60~80% ethanol carries out 30~60min of subcritical abstraction in 90~120 DEG C, obtains Tongkat Ali alcohol extraction liquid, wherein, should
The mass ratio of Tongkat Ali powder and alcohol solvent is 1：5-10；
（2）Concentration：It is the Tongkat Ali ethanol to be concentrated in vacuo after above-mentioned Tongkat Ali alcohol extraction liquid is cooled to room temperature
The 10%-20% of extract, obtains concentrate；
（3）Centrifugation：Gained concentrate is subjected to sleeping spiral shell centrifugation, obtains centrifuged supernatant；
（4）Resin chromatography：By macroporous resin column on gained supernatant, gradient elution, eluent is obtained；
（5）Condensing crystallizing：Gained eluent is concentrated, adds alcohol to crystallize, filters, obtains filtrate；
（6）Decolouring crystallizing and drying：The ethanol that volume fraction is 30% is added in gained filtrate and dilutes 8~10 times, must be diluted
Liquid, activated carbon decolorizing is then added in the dilution, filtering, concentration, crystallization, vacuum drying, obtains eurycomanone.
Above-mentioned steps（2）The temperature of middle concentration is 60~80 DEG C, vacuum is -0.1~-0.07MPa.
Above-mentioned steps（3）In centrifugal rotational speed be 3000-3500r/min.
Above-mentioned steps（4）In macroreticular resin be HPD100 resins, gradient elution refers to first with the second that volume fraction is 10%
Alcohol elute 1BV, then with volume fraction be 30% ethanol elution 2.5BV, finally with volume fraction be 60%~80% ethanol elution
3~4BV.
Above-mentioned steps（5）Volume after middle concentration is the 1/500~1/1000 of effluent volume；The addition of alcohol is dense
0.5~1 times of contracting liquid product；The temperature of crystallization is room temperature, and the time is 1~2h.
Above-mentioned steps（6）The addition of middle activated carbon is the 2-4%, bleaching time 1-2h of dilution weight；Cycles of concentration
For 10-20 times；The temperature of crystallization is 2-7 DEG C, time 24-48h；Vacuum drying temperature is 60~70 DEG C.
The present invention is Malay Tongkat Ali raw material from the place of production, and its eurycomanone content is more than 0.1%, for producing
Yield can be improved, simplifies technique, reduces production cost；Active ingredient dissolution rate can not only be improved using subcritical abstraction technology
With the utilization rate of Tongkat Ali, extraction time is shortened, moreover it is possible to prevent active ingredient oxidation, improve yield；It is big using HPD100
Macroporous adsorbent resin, cheap, quantity of sample handling is big, reduces production cost；Organic solvent ethanol only is used in this technique, it is whole
Individual process greenization.This technique simply continuous operation property is strong, is adapted to large-scale industrial production, using eurycomanone obtained by this technique
High purity 98%, ultimate yield be more than 90%.
Brief description of the drawings
Fig. 1 is the high-efficient liquid phase chromatogram of the gained eurycomanone product of present example 1；Wherein, ordinate represents ultraviolet suction
Receive, abscissa is the time.
Embodiment
Tongkat Ali raw material used in following each embodiments is commercial products, and the place of production is Malaysian, in the Tongkat Ali
Eurycomanone content is 0.113%.
Gained eurycomanone product is detected using high performance liquid chromatography in following each embodiments, and testing conditions are as follows：
Chromatographic column：C18 posts（4.6*250mm）, Detection wavelength：240nm, solvent：Methanol, flow velocity：1ml/min, column temperature：30
DEG C, sample size：10ul, mobile phase：The phosphate aqueous solution of acetonitrile -0.1%, gradient elution ratio are followed successively by 5/95,20/80,5/92.
Embodiment 1
Take 4kg Tongkat Alis to crush, be fitted into subcritical abstraction kettle, with the alcohol solvent that volume fraction is 60% in 90 DEG C
The mass ratio of progress subcritical abstraction 60min, Tongkat Ali powder and alcohol solvent is 1：5, obtain Tongkat Ali alcohol extraction liquid；Will
The Tongkat Ali alcohol extraction liquid is cooled to room temperature, is to be concentrated under -0.1MPa in 60 DEG C, vacuum, the volume after concentration
For the 20% of the Tongkat Ali alcohol extraction liquid, concentrate is obtained；Gained concentrate is subjected to sleeping spiral shell centrifugation with 3000r/min, obtain from
Supernatant；By HPD100 macroporous resin columns, gradient elution on gained supernatant（First with the ethanol elution that volume fraction is 10%
1BV, then with volume fraction be 30% ethanol elution 2.5BV, finally with volume fraction be 60% ethanol elution 4BV）, must elute
Liquid；It is the 1/500 of effluent volume by the concentration of gained eluent, obtains elution concentrate, be incorporated as washing in the elution concentrate
The alcohol of de- 0.5 times of the volume of concentrate, crystallizes 2h at room temperature, filters, and crystal is eluted totally with a small amount of absolute ethyl alcohol, must be filtered
Liquid；The ethanol that volume fraction is 30% is added in the filtrate and dilutes 8 times, dilution is obtained, is then incorporated as in the dilution dilute
The activated carbon decolorizing 2h of liquid weight 2% is released, filtering, 10 times of concentration, 48h, 60 DEG C of vacuum drying is crystallized in 2 DEG C, it is yellowish to obtain 4.19g
Color powder, is detected through high performance liquid chromatography（Chromatogram is as shown in Figure 1）, eurycomanone appearance time is 15.837min, eurycomanone
Purity is 98.27%, ultimate yield 91.10%.
Embodiment 2
Take 4kg Tongkat Alis to crush, be fitted into subcritical abstraction kettle, be the alcohol solvent that volume fraction is 70% with concentration
In 100 DEG C of progress subcritical abstraction 45min, the mass ratio of Tongkat Ali powder and alcohol solvent is 1：8, obtain Tongkat Ali ethanol extraction
Take liquid；The Tongkat Ali alcohol extraction liquid is cooled to room temperature, be to be concentrated under -0.08MPa in 70 DEG C, vacuum, concentrate
Volume afterwards is the 15% of the Tongkat Ali alcohol extraction liquid, obtains concentrate；Gained concentrate is subjected to sleeping spiral shell with 3200r/min
Centrifugation, obtains centrifuged supernatant；By HPD100 macroporous resin columns, gradient elution on gained supernatant（It is first 10% with volume fraction
Ethanol elution 1BV, then with volume fraction be 30% ethanol elution 2.5BV, finally with volume fraction be 70% ethanol elution
3.5BV）, obtain eluent；It is the 1/800 of effluent volume by the concentration of gained eluent, obtains elution concentrate, is concentrated in the elution
It is incorporated as eluting the alcohol of 0.8 times of the volume of concentrate in liquid, crystallizes 1.5h at room temperature, filter, by crystal anhydrous second on a small quantity
Alcohol elution is clean, obtains filtrate；The ethanol that volume fraction is 30% is added in the filtrate and dilutes 9 times, dilution is obtained, then in this
Be incorporated as the activated carbon decolorizing 1.5h of dilution weight 3% in dilution, filtering, 15 times of concentration, crystallize in 5 DEG C 36h, 65 DEG C it is true
Sky is dried, and is obtained 4.29g pale yellow powders, is detected through high performance liquid chromatography, and eurycomanone appearance time is 15.839min, wide tassel
Ketone purity is 98.33%, ultimate yield 93.33%.
Embodiment 3
Take 4kg Tongkat Alis to crush, be fitted into subcritical abstraction kettle, be the alcohol solvent that volume fraction is 80% with concentration
In 120 DEG C of progress subcritical abstraction 30min, the mass ratio of Tongkat Ali powder and alcohol solvent is 1：10, obtain Tongkat Ali ethanol
Extract；The Tongkat Ali alcohol extraction liquid is cooled to room temperature, be to be concentrated under -0.07MPa in 80 DEG C, vacuum, it is dense
Volume after contracting is the 10% of the Tongkat Ali alcohol extraction liquid, obtains concentrate；Gained concentrate is crouched with 3500r/min
Spiral shell centrifuges, and obtains centrifuged supernatant；By HPD100 macroporous resin columns, gradient elution on gained supernatant（It is first 10% with volume fraction
Ethanol elution 1BV, then with volume fraction be 30% ethanol elution 2.5BV, finally with volume fraction be 80% ethanol elution
3BV）, obtain eluent；It is the 1/1000 of effluent volume by the concentration of gained eluent, obtains elution concentrate, is concentrated in the elution
It is incorporated as eluting the alcohol of 1 times of the volume of concentrate in liquid, crystallizes 1h at room temperature, filters, crystal is drenched with a small amount of absolute ethyl alcohol
Wash clean, obtain filtrate；The ethanol that volume fraction is 30% is added in the filtrate and dilutes 10 times, dilution is obtained, then in the dilution
The activated carbon decolorizing 1h of dilution weight 4% is incorporated as in liquid, filtering, 20 times of concentration, 24h, 70 DEG C of vacuum drying are crystallized in 7 DEG C,
4.15g pale yellow powders are obtained, are detected through high performance liquid chromatography, eurycomanone appearance time is 15.841min, and eurycomanone purity is
98.17%, ultimate yield 90.13%.
Claims (10)
1. a kind of technique of the rapid extraction eurycomanone from Tongkat Ali, it is characterised in that the processing step is as follows：
(1) subcritical abstraction：Using Tongkat Ali as raw material, with the ethanol that volume fraction is 60~80% in 90~120 after crushing
DEG C 30~60min of subcritical abstraction is carried out, obtain Tongkat Ali alcohol extraction liquid, wherein, the Tongkat Ali powder and alcohol solvent
Mass ratio is 1：5-10；
(2) concentrate：Above-mentioned Tongkat Ali alcohol extraction liquid is cooled to be concentrated in vacuo after room temperature and extracted for the Tongkat Ali ethanol
The 10%-20% of liquid, obtains concentrate；
(3) centrifuge：Gained concentrate is subjected to sleeping spiral shell centrifugation, obtains centrifuged supernatant；
(4) resin chromatography：By HPD100 macroporous resin columns on gained supernatant, gradient elution, eluent is obtained；
(5) condensing crystallizing：Gained eluent is concentrated, adds alcohol to crystallize, filters, obtains filtrate；
(6) decolouring crystallizing and drying：The ethanol that volume fraction is 30% is added in gained filtrate and dilutes 8~10 times, obtains dilution,
Then activated carbon decolorizing is added in the dilution, filtering, concentration, crystallization, vacuum drying, obtains eurycomanone.
A kind of 2. technique of the rapid extraction eurycomanone from Tongkat Ali as claimed in claim 1, it is characterised in that：The step
Suddenly the temperature being concentrated in vacuo in (2) is 60~80 DEG C, vacuum is -0.1~-0.07MPa.
A kind of 3. technique of the rapid extraction eurycomanone from Tongkat Ali as claimed in claim 1, it is characterised in that：The step
Suddenly the rotating speed of centrifugation is 3000-3500r/min in (3).
A kind of 4. technique of the rapid extraction eurycomanone from Tongkat Ali as claimed in claim 1, it is characterised in that：The step
Suddenly the gradient elution in (4) refer to first with volume fraction be 10% ethanol elution 1BV, then with volume fraction be 30% ethanol
2.5BV is eluted, finally with 3~4BV of ethanol elution that volume fraction is 60%~80%.
A kind of 5. technique of the rapid extraction eurycomanone from Tongkat Ali as claimed in claim 1, it is characterised in that the step
Suddenly the volume after being concentrated in (5) is the 1/500~1/1000 of effluent volume.
A kind of 6. technique of the rapid extraction eurycomanone from Tongkat Ali as claimed in claim 1, it is characterised in that the step
Suddenly the addition of alcohol is 0.5~1 times of the volume of concentrate in (5).
A kind of 7. technique of the rapid extraction eurycomanone from Tongkat Ali as claimed in claim 1, it is characterised in that the step
Suddenly the temperature of crystallization is room temperature in (5), and the time is 1~2h.
A kind of 8. technique of the rapid extraction eurycomanone from Tongkat Ali as claimed in claim 1, it is characterised in that：The step
Suddenly the addition of activated carbon is the 2-4%, bleaching time 1-2h of dilution weight in (6).
A kind of 9. technique of the rapid extraction eurycomanone from Tongkat Ali as claimed in claim 1, it is characterised in that：The step
Suddenly the temperature of crystallization is 2-7 DEG C in (6), time 24-48h.
A kind of 10. technique of the rapid extraction eurycomanone from Tongkat Ali as claimed in claim 1, it is characterised in that：It is described
Vacuum drying temperature is 60~70 DEG C in step (6).
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Families Citing this family (5)
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| CN107353296B (en) * | 2017-07-06 | 2019-03-29 | 湖南华诚生物资源股份有限公司 | A method of extracting activated protein and eurycomanone from Tongkat Ali |
| CN109535172B (en) * | 2018-10-19 | 2020-06-05 | 广东省农业科学院果树研究所 | Quassia amara picrorhiza compounds and application thereof in preparation of insect antifeedant |
| CN110749680A (en) * | 2019-11-12 | 2020-02-04 | 福建省微生物研究所 | Method for rapidly identifying Eurycoma longifolia chemical components |
| CN111303180A (en) * | 2020-02-21 | 2020-06-19 | 湖南中茂生物科技有限公司 | Method for extracting eurycomanone from eurycoma longifolia |
| CN113197923A (en) * | 2021-05-11 | 2021-08-03 | 湘南学院 | Eurycoma longifolia extract and application thereof in medicines for preventing and treating prostatitis |
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| CN103408564B (en) * | 2013-08-16 | 2016-03-16 | 李玉山 | The extraction and purification process of eurycomanone in Tongkat Ali plant |
| CN106366092B (en) * | 2016-08-29 | 2018-09-04 | 湖南华诚生物资源股份有限公司 | A kind of industrial production process detaching eurycomanone from Tongkat Ali |
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