CN109942657A - A method of extracting dehydrobenzene from sweet potato - Google Patents
A method of extracting dehydrobenzene from sweet potato Download PDFInfo
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Abstract
The method that the invention discloses a kind of from sweet potato extracts dehydrobenzene, including pre-inversion processing, sour water solution and extraction, purifying.The present invention for classical acid hydrolysis can not combining Dioscin be kept completely separate with cellulose, the defect for causing efficiency of pcr product very low, by the way that sweet potato paste is stirred with treatment fluid, make the abundant swollen of its cellulose and the hydrogen bond and glycosides key for combining sweet potato cellulose with Dioscin after mechanical lapping processing are broken, Dioscin is promoted to separate, to improve the recovery rate of subsequent acid-hydrolyzed rate and DHEA, achieve the purpose that DHEA in quick, high efficiency extraction sweet potato.
Description
Technical field
The present invention relates to the extracting methods of dehydrobenzene, and the method for dehydrobenzene is extracted especially from sweet potato.
Background technique
Dehydrobenzene (DHEA) is most one of the hormone of people's in-vivo content, has anti-aging, antitumor, inhibition fertilizer
It is fat, adjust the effects of human hormone, while being also the intermediate for manufacturing steroid hormone class drug.Natural plant containing DHEA
Object is less, and wherein sweet potato is content one kind more abundant.
DHEA is mainly present in plant cell wall in conjunction with cellulose in the form of Dioscin in sweet potato, from sweet potato
The common method of middle extraction DHEA is acid-hydrolysis method, but because of presence of combining closely such as cellulose in Dioscin and sweet potato, biography
System acid-hydrolysis method can not combining Dioscin be kept completely separate with cellulose, therefore the recovery rate of conventional method gained sweet potato DHEA
It is lower and take a long time, low efficiency.For this purpose, Yao Juying etc. is conducive to by the way that sweet potato is carried out spontaneous fermentation processing before hydrolysis
Product yield is improved, yield is up to 5/10000ths, but this method takes a long time, and only fermentation will carry out two days, and ferment
Journey is uncontrollable, leads to unstable product quality.
Summary of the invention
The purpose of the present invention is for the prior art is defective, provide a kind of side that dehydrobenzene is extracted from sweet potato
Method, it is intended to improve the yield of dehydrobenzene and shorten extracting cycle.
Above-mentioned purpose is realized by using following technical scheme:
A method of extracting dehydrobenzene from sweet potato, comprising the following steps:
1) by fresh sweet potato washing impurity elimination, the treatment fluid of 10-40% weight, room temperature condition are added into sweet potato paste for mashing
Lower stirring 1-5h, then with water by sweet potato plasm scouring to neutrality, the water that 1-2 times of weight is added after filtering into sweet potato paste again is used in combination
Colloid mill grinds 10-100min, is centrifuged, water-bath 8-24h under the conditions of gained is deposited in 50-80 DEG C,
The treatment fluid is highly basic, urea, inorganic mixed salt solution, highly basic in the mixed solution, urea, inorganic salts
Weight concentration is respectively 5-10%, 5-10%, 1-5%；
2) the dense H of 1-5% weight is then added into precipitating2SO4, 8-16h is hydrolyzed under the conditions of 80-100 DEG C, is cooled to
After room temperature, pH is adjusted to neutrality with NaOH solution, centrifugation takes precipitating；
3) petroleum ether of 5-10 times of weight is added into precipitating obtained by step 2), ultrasound extracts 0.5-2h, filtering, and collection mentions
It takes liquid and is concentrated under reduced pressure；
4) it by silicagel column on concentrate, is eluted with non-polar organic solvent, collects eluent, after spray drying to obtain the final product
Dehydrobenzene.
Preferably, the highly basic is at least one of potassium hydroxide, sodium hydroxide, lithium hydroxide.
Preferably, the inorganic salts are at least one of zinc salt, calcium salt, molysite, magnesium salts.
Preferably, the non-polar organic solvent is acetone and petroleum ether mixed solution.
It is further preferred that the volume ratio of the acetone and petroleum ether is 0.5-5:1.
According to one embodiment of present invention, the optimal technical solution of effect are as follows:
1) by fresh sweet potato washing impurity elimination, the treatment fluid of 20% weight is added into sweet potato paste, stirs under room temperature for mashing
4h is mixed, then with water by sweet potato plasm scouring to neutrality, the water blend compounds body mill of 1.6 times of weight is added after filtering into sweet potato paste again
30min is ground, is centrifuged, water-bath 12h under the conditions of gained is deposited in 60 DEG C,
The treatment fluid is NaOH, urea, CaCl2Mixed solution, NaOH, urea, CaCl in the mixed solution2Weight
Measuring concentration is respectively 8%, 8%, 3%；
2) the dense H of 2% weight is then added into precipitating2SO4, 12h is hydrolyzed under the conditions of 90 DEG C, after being cooled to room temperature, is used
NaOH solution adjusts pH to neutrality, and centrifugation takes precipitating；
3) petroleum ether of 8 times of weight, ultrasound extraction 1h are added into precipitating obtained by step 2), filtering collects extracting solution simultaneously
It is concentrated under reduced pressure；
4) it by silicagel column on concentrate, is eluted with acetone and petroleum ether mixed solution (volume ratio 1:1), collection is washed
De- liquid, up to dehydrobenzene after spray drying.
The beneficial effects of the present invention are:
The present invention for classical acid hydrolysis can not combining Dioscin be kept completely separate with cellulose, lead to efficiency of pcr product
Very low defect makes the abundant swollen of its cellulose and after mechanical lapping processing by the way that sweet potato paste to be stirred with treatment fluid
Hydrogen bond and glycosides the key fracture for combining sweet potato cellulose with Dioscin, promote Dioscin to separate, thus
The recovery rate for improving subsequent acid-hydrolyzed rate and DHEA achievees the purpose that DHEA in quick, high efficiency extraction sweet potato.With it is existing
Fermentation pretreatment compare, pretreatment time of the present invention is shorter, and process conditions are more controllable, and product quality is more stable.
The present invention improves the recovery rate of sweet potato DHEA and shortens extracting cycle.
Specific embodiment
The present invention is described in detail below by specific embodiment.
Embodiment 1
A method of extracting dehydrobenzene from sweet potato, steps are as follows:
1) pre-inversion is handled:
By fresh sweet potato washing impurity elimination, the treatment fluid of 20% weight is added into sweet potato paste for mashing, and constant temperature stirs at 8 DEG C
The water blend compounds body barreling of 1.6 times of weight is added then with water by sweet potato plasm scouring to neutrality in 4h into sweet potato paste again after filtering
30min is ground, centrifugation, water-bath 12h under the conditions of gained is deposited in 60 DEG C, the main function of water-bath is to make a part of furan sterol saponin
Enzymatic hydrolysis is converted into spiral shell sterol saponin, and the latter is easier to be converted into diosgenin, to further increase saponin yield.
The treatment fluid is NaOH, urea, CaCl2Mixed solution, NaOH, urea, CaCl in the mixed solution2Weight
Measuring concentration is respectively 8%, 8%, 3%.
2) sour water solution:
Then the dense H of 2% weight is added into precipitating2SO4, 12h is hydrolyzed under the conditions of 90 DEG C, after being cooled to room temperature, is used
NaOH solution adjusts pH to neutrality, and centrifugation takes precipitating.Acid-hydrolyzed main function is to obtain diosgenin, in conventional method
The step takes a long time and acidolysis is incomplete, and hydrolysis temperature is excessively high and the too long easy initiation safety problem of hydrolysis time.
3) it extracts:
The petroleum ether of 8 times of weight, ultrasound extraction 1h are added into precipitating obtained by step 2), filtering is collected extracting solution and subtracted
Pressure concentration.The purpose of ultrasound extraction is mechanical effect, cavitation effect and the fuel factor having using ultrasonic wave, by increasing medium
The movement velocity of molecule increases the penetration power of medium sufficiently to extract biological effective components.
4) it purifies:
It by silicagel column on concentrate, is eluted with acetone and petroleum ether mixed solution (volume ratio 1:1), collects elution
Liquid, up to dehydrobenzene after spray drying.
Embodiment 2
A method of extracting dehydrobenzene from sweet potato, steps are as follows:
1) by fresh sweet potato washing impurity elimination, mashing the treatment fluid of 15% weight is added into sweet potato paste, constant temperature stirs at 0 DEG C
5h is mixed, then with water by sweet potato plasm scouring to neutrality, the water blend compounds body barreling of 2 times of weight is added after filtering into sweet potato paste again
Grind 60min, centrifugation, water-bath 8h under the conditions of gained is deposited in 80 DEG C.
The treatment fluid is lithium hydroxide, urea, ZnCl2Mixed solution, lithium hydroxide in the mixed solution, urea,
ZnCl2Weight concentration be respectively 5%, 10%, 5%.
2) the dense H of 3% weight is then added into precipitating2SO4, 16h is hydrolyzed under the conditions of 80 DEG C, after being cooled to room temperature, is used
NaOH solution adjusts pH to neutrality, and centrifugation takes precipitating.
3) petroleum ether of 5 times of weight, ultrasound extraction 2h are added into precipitating obtained by step 2), filtering collects extracting solution simultaneously
It is concentrated under reduced pressure.
4) it by silicagel column on concentrate, is eluted, is collected with acetone and petroleum ether mixed solution (volume ratio 0.5:1)
Eluent, up to dehydrobenzene after spray drying.
Embodiment 3
A method of extracting dehydrobenzene from sweet potato, steps are as follows:
1) by fresh sweet potato washing impurity elimination, mashing the treatment fluid of 40% weight is added into sweet potato paste, constant temperature stirs at 5 DEG C
2h is mixed, then with water by sweet potato plasm scouring to neutrality, the water blend compounds body barreling of 1 times of weight is added after filtering into sweet potato paste again
10min is ground, centrifugation, water-bath is for 24 hours under the conditions of gained is deposited in 50 DEG C.
The treatment fluid is potassium hydroxide, urea, MgCl2Mixed solution, potassium hydroxide in the mixed solution, urea,
MgCl2Weight concentration be respectively 10%, 7%, 2%.
2) the dense H of 1% weight is then added into precipitating2SO4, 8h is hydrolyzed under the conditions of 100 DEG C, after being cooled to room temperature, is used
NaOH solution adjusts pH to neutrality, and centrifugation takes precipitating.
3) petroleum ether of 10 times of weight, ultrasound extraction 0.5h are added into precipitating obtained by step 2), extracting solution is collected in filtering
And it is concentrated under reduced pressure.
4) it by silicagel column on concentrate, is eluted with acetone and petroleum ether mixed solution (volume ratio 5:1), collection is washed
De- liquid, up to dehydrobenzene after spray drying.
Embodiment 4
A method of extracting dehydrobenzene from sweet potato, steps are as follows:
1) by fresh sweet potato washing impurity elimination, mashing the treatment fluid of 30% weight is added into sweet potato paste, constant temperature stirs at 3 DEG C
1h is mixed, then with water by sweet potato plasm scouring to neutrality, the water blend compounds body mill of 1.5 times of weight is added after filtering into sweet potato paste again
Grind 100min, centrifugation, water-bath 18h under the conditions of gained is deposited in 70 DEG C.
The treatment fluid is NaOH, urea, CaCl2Mixed solution, NaOH, urea, CaCl in the mixed solution2Weight
Measuring concentration is respectively 6%, 10%, 2%.
2) the dense H of 5% weight is then added into precipitating2SO4, 16h is hydrolyzed under the conditions of 90 DEG C, after being cooled to room temperature, is used
NaOH solution adjusts pH to neutrality, and centrifugation takes precipitating.
3) petroleum ether of 6 times of weight, ultrasound extraction 1.5h are added into precipitating obtained by step 2), extracting solution is collected in filtering
And it is concentrated under reduced pressure.
4) it by silicagel column on concentrate, is eluted with acetone and petroleum ether mixed solution (volume ratio 2:1), collection is washed
De- liquid, up to dehydrobenzene after spray drying.
By sample progress HPLC quantitative detection prepared by embodiment 1-4: sample crosses 0.45 μM of filter membrane after being redissolved with acetonitrile, adopts
With C18 chromatographic column, mobile phase is acetonitrile: water=7:3, Detection wavelength 210nm, 40 DEG C of column temperature, flow velocity 1.0mL/min, sample introduction body
10 μ L, DHEA content in external standard method sample are accumulated, and recovery rate, knot are calculated according to the DHEA content in sample and raw material sweet potato
Fruit see the table below 1.
DHEA content and recovery rate in 1 embodiment 1-4 sample of table
| Sample size (%) | Recovery rate (%) | |
| Embodiment 1 | 96.7 | 0.055 |
| Embodiment 2 | 96.2 | 0.048 |
| Embodiment 3 | 95.4 | 0.045 |
| Embodiment 4 | 95.8 | 0.052 |
Claims (5)
1. a kind of method for extracting dehydrobenzene from sweet potato, it is characterised in that the following steps are included:
1) by fresh sweet potato washing impurity elimination, the treatment fluid of 10-40% weight is added into sweet potato paste, stirs under room temperature for mashing
1-5h is mixed, then with water by sweet potato plasm scouring to neutrality, the water blend compounds body of 1-2 times of weight is added after filtering into sweet potato paste again
Mill grinding 10-100min, centrifugation, water-bath 8-24h under the conditions of gained is deposited in 50-80 DEG C,
The treatment fluid is highly basic, urea, inorganic mixed salt solution, the weight of highly basic, urea, inorganic salts in the mixed solution
Concentration is respectively 5-10%, 5-10%, 1-5%；
2) the dense H of 1-5% weight is then added into precipitating2SO4, 8-16h is hydrolyzed under the conditions of 80-100 DEG C, is cooled to room temperature
Afterwards, pH is adjusted to neutrality with NaOH solution, centrifugation takes precipitating；
3) petroleum ether of 5-10 times of weight, ultrasound extraction 0.5-2h are added into precipitating obtained by step 2), extracting solution is collected in filtering
And it is concentrated under reduced pressure；
4) it by silicagel column on concentrate, is eluted with non-polar organic solvent, collects eluent, up to dehydrogenation after spray drying
Epiandrosterone.
2. the method for dehydrobenzene is extracted from sweet potato as described in claim 1, it is characterised in that: the highly basic is hydroxide
At least one of potassium, sodium hydroxide, lithium hydroxide.
3. the method for dehydrobenzene is extracted from sweet potato as described in claim 1, it is characterised in that: the inorganic salts are zinc
At least one of salt, calcium salt, molysite, magnesium salts.
4. the method for dehydrobenzene is extracted from sweet potato as described in claim 1, it is characterised in that: the nonpolarity is organic molten
Agent is acetone and petroleum ether mixed solution.
5. the method for dehydrobenzene is extracted from sweet potato as claimed in claim 4, it is characterised in that: the acetone and petroleum ether
Volume ratio be 0.5-5:1.
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Cited By (3)
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| CN111944869A (en) * | 2020-08-03 | 2020-11-17 | 湖北省农业科学院农产品加工与核农技术研究所 | Preparation method of dehydroepiandrosterone |
| CN112021563A (en) * | 2020-07-24 | 2020-12-04 | 湖北省农业科学院农产品加工与核农技术研究所 | Preparation method of sweet potato whole powder rich in free dehydroepiandrosterone |
| CN112167618A (en) * | 2020-06-29 | 2021-01-05 | 武汉林宝莱生物科技有限公司 | Dehydroepiandrosterone health food and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112021563B (en) * | 2020-07-24 | 2022-08-09 | 湖北省农业科学院农产品加工与核农技术研究所 | Preparation method of sweet potato whole powder rich in free dehydroepiandrosterone |
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| CN111944869B (en) * | 2020-08-03 | 2021-09-28 | 湖北省农业科学院农产品加工与核农技术研究所 | Preparation method of dehydroepiandrosterone |
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