CN103319561B - A kind of method extracting plant sterol and cerosin from Sugarcane peel. - Google Patents

A kind of method extracting plant sterol and cerosin from Sugarcane peel. Download PDF

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CN103319561B
CN103319561B CN201310245316.2A CN201310245316A CN103319561B CN 103319561 B CN103319561 B CN 103319561B CN 201310245316 A CN201310245316 A CN 201310245316A CN 103319561 B CN103319561 B CN 103319561B
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plant sterol
cerosin
extraction
sugarcane
extract
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CN103319561A (en
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罗自生
冯思敏
张炎冰
钟舟
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Zhejiang University ZJU
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Zhejiang University ZJU
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/74Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

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Abstract

The invention discloses a kind of method extracting plant sterol and cerosin from Sugarcane peel., comprising: get Sugarcane peel., dry, pulverize obtained powder; Described powder is placed in ethanol lixiviate for some time, filters, collect filtrate and filter residue; Extract from described filtrate and obtain plant sterol, from described filter residue, utilize normal hexane refluxing extraction to obtain cerosin.The present invention take Sugarcane peel. as raw material, and raw material sources are wide, have no side effect, can obtain plant sterol and cerosin simultaneously, and production technique is simple, and first extract sugarcane fat and refined plant sterol by the method for fractional steps, rear extraction cerosin, effectively reduces solvent consumption.In addition, plant sterol and the sugar-cane wax yield of method extraction of the present invention are high, and yield is higher can reach 2.17 ‰ ~ 2.88 ‰ and 5.16% ~ 6.28% respectively.

Description

A kind of method extracting plant sterol and cerosin from Sugarcane peel.
Technical field
The present invention relates to biological technical field, particularly relate to a kind of method extracting plant sterol and cerosin from Sugarcane peel..
Background technology
Plant sterol is a steroid-like of occurring in nature, belongs to the secondary alcohol of saturated (or unsaturated).Plant sterol is the required composition of stable plant cell membrane, and similar with cholesterol effect in animal body, it is distributed widely in vegetables oil, seed, nut, vegetables and fruit.Plant sterol has many physiological functions, wherein the most strikingly decreasing cholesterol effect.In addition, plant sterol at Tumor suppression, prevent and treat in heart trouble, anticancer, immunity moderation function etc. and also all play an important role, be described as " key of life " by scientific circles.
At present, mainly the extracting from soybean oil, vegetable seeds wet goods deodorization distillate of plant sterol.US Patent No. 5117015 is reported, use special solvent system from deodorization distillate, obtain the Stigmasterol product concentrated, total sterol content from 10% ~ 15%(wherein Stigmasterol account for 17% ~ 19%) bring up to 85% ~ 96%(wherein Stigmasterol account for 20% ~ 25%).
Present stage, the technique extracting plant sterol from the filter mud of cane sugar manufacture factory all has related article to report at home and abroad, but directly from Sugarcane peel. extraction and application rarely have report.
Sugar-cane wax is the wax on sugarcane epidermis, and sugar-cane wax contains based on the physiologically active substance of long-chain (C20-C30) high fatty alcohol.Cerosin is proved to be to obtain one of optimal raw material of octacosanol, and Li Xiaoguang etc. are once described a kind of method from alcohols high purity octacosanol in CN1297873A Chinese patent at publication number.Crude cane wax is the mixture of true wax and fatty lipoids, the removing of soft fatty substance just can must be obtained the refined cane wax similar with other vegetable wax.The method of bibliographical information extraction cerosin mostly is extracts crude cane wax with organic solvents such as benzene, toluene, sherwood oil, gasoline, trieline, Ethylene Dichloride, tetracol phenixin, gasoline and alcohol mixed solutions from filter mud, after use organic solvent (acetone, Virahol) refining removing fatty substance, refined cane wax.He Wei's equality people in 1992, utilizes sherwood oil-ethanolic soln to extract crude cane wax, and rear organic solvent (acetone, Virahol) twice refining removing fatty substance, refined cane wax is up to 5.8%.2011 old catches up with Lin Dengren, and by mixed solvent water bath reflux method and ultrasonic-assisted extraction method, extract with the alcohol-gasoline mixed solvent of 70% ethanol content, purifying cerosin productive rate can reach 4.6%.But there is following defect: (1), for refining solvent as acetone etc., volatilization is strong, is unfavorable for safety in production; (2) portion of reagent as with high costs in Virahol, reclaim unfavorable, be not suitable for scale operation.
In addition, the kind based on material contained in raw material is different, and the restriction of extraction process, and at present, the preparation of plant sterol and cerosin is all extract respectively by independent production technique, and extraction cost is expensive.
Summary of the invention
The invention provides a kind of method extracting plant sterol and cerosin from Sugarcane peel., take Sugarcane peel. as raw material, can obtain plant sterol and cerosin simultaneously, and production technique is simple, and security is high and yield is high.
From Sugarcane peel., extract a method for plant sterol and cerosin, comprising:
(1) get Sugarcane peel., dry, pulverize obtained powder;
(2) described powder is placed in ethanol lixiviate for some time, filters, collect filtrate and filter residue;
(3) from described filtrate, extraction obtains plant sterol, utilizes normal hexane refluxing extraction to obtain cerosin from described filter residue.
Sugarcane fat is dissolved in cold ethanol, and cerosin is insoluble, and therefore by alcohol steep, sugarcane fat is present in filtrate, and cerosin is present in filter residue, achieves being separated of sugarcane fat and cerosin.The extraction of plant sterol and cerosin is carried out again respectively for filtrate and filter residue.Ethanol is lixiviate reagent, can adopt ethanol or the dehydrated alcohol of 95%, if without specified otherwise in the present invention, all refer to dehydrated alcohol.
During alcohol steep, liquid ratio is 8 ~ 4: 1, is preferably 6 ~ 5: 1, is more preferably 5: 1.Along with the increase of liquid ratio, the concentration difference of intraor extracellular sugarcane fat is larger, and mass transfer force is large, is conducive to the leaching of sugarcane fat, but the excessive waste not only causing reagent of solid-liquid ratio, the complicacy of subsequent filtrate evaporate to dryness after also increasing.
It will be understood by those in the art that lixiviate liquid ratio is often referred to the volume mass ratio (ml: g) of lixiviate reagent and material.
Suitable extraction time and temperature are conducive to sugarcane fat and realize effectively being separated with cerosin, and ensure that sugarcane fat is fully separated out, and improve the yield of plant sterol and cerosin.Preferably, extraction temperature is 30 ~ 35 DEG C, and extraction time is 4 ~ 8 hours.Extraction temperature is too high, then cerosin is easily separated out and affects the separation of cerosin, sugarcane fat, and extraction temperature is too low, then molecular motion is slow, affects sugarcane fat precipitation rate; And extraction time is too short, may cause having part sugarcane fat not leach, extraction time is long, then can increase the leaching content of impurity, finally affects purity, the yield of plant sterol and cerosin.
The extracting method of described plant sterol is: get described filtrate, evaporate to dryness, adds alkali and carries out saponification reaction, add extraction agent and extract, get oil phase after reacting completely, and evaporate to dryness obtains plant sterol.
In step (1), the temperature of described filtrate when evaporate to dryness is 40 ~ 50 DEG C.
During saponification, alkali is preferably the aqueous solution of potassium hydroxide or the ethanolic soln of potassium hydroxide, and concentration is 2 ~ 4mol/L, and the consumption of potassium hydroxide is 2 ~ 10% of sugarcane fat weight.
The temperature of described saponification is 80 ~ 90 DEG C, and the time is 2 ~ 4 hours, and preferably, the time of saponification is 2 hours.
For improving the yield of plant sterol, before extraction, add metallic compound precipitator and precipitate in reaction solution, described metallic compound precipitator is monovalence or polyvalent metal salt, preferred Repone K.According to the similar principle that mixes, the ionic concn that Repone K can improve aqueous phase makes polarity improve, and plant sterol is more prone to separate out from aqueous phase enter in petroleum ether layer, and Repone K can be dissolved in rapidly above-mentioned reaction solution.
During petroleum ether extraction, each consumption of sherwood oil is 1 ~ 2 times of former Sugarcane peel. quality, and extraction times is generally 2 ~ 3 times.
Cerosin can extract by normal hexane from filter residue, and during refluxing extraction, liquid ratio 6 ~ 8: 1, is preferably 7 ~ 8: 1.
The temperature and time of refluxing extraction affects extraction efficiency and the purity of cerosin, and the temperature of described refluxing extraction is 70 ~ 80 DEG C, and the time is 2 ~ 3h.
Cerosin of the present invention be fusing point between 76 ~ 82 DEG C, be not containing the hard cerosin of sugarcane fat.
Compared with prior art, beneficial effect of the present invention is:
(1) the present invention take Sugarcane peel. as raw material, and raw material sources are wide, have no side effect, can obtain plant sterol and cerosin simultaneously.
(2) production technique of the present invention is simple, and first extract sugarcane fat and refined plant sterol by the method for fractional steps, rear extraction cerosin, effectively reduces solvent consumption.
(3) plant sterol that extracts of method of the present invention and cerosin yield high, the yield of plant sterol can reach 2.17 ‰-2.88 ‰, can refine further and develop β-sitosterol, the high purity sterol monomers such as Stigmasterol; Cerosin adopts normal hexane refluxing extraction, and yield can reach 5.16%-6.28%.In addition, sugar-cane wax outward appearance prepared by the present invention has conventional plant wax feature, is the hard cerosin not containing sugarcane fat, can refine exploitation policosanol further.
(4) solvent for use ethanol and normal hexane in leaching process of the present invention, sherwood oil kind is single is easy to get, security is high.
Embodiment
Below in conjunction with specific embodiment, the present invention is further explained.
Embodiment 1
(1), after Sugarcane peel. being dried pulverizing at 30 DEG C, this powder 5g 25mL alcohol is taken 30 DEG C of lixiviates 8 hours, suction filtration;
(2) gained filtrate obtains sugarcane fat after 40 DEG C of evaporates to dryness, and the gained sugarcane fat ethanolic soln of 5mL2mol/L potassium hydroxide is hydrolyzed saponification 2 hours at 80 DEG C;
(3) add 1g Repone K toward saponification liquor after hydrolysis, and use 10mL petroleum ether extraction unsaponifiables 3 times at every turn, this solution evaporate to dryness is obtained plant sterol;
(4) by (1) gained filter residue 35mL normal hexane solvent (liquid ratio is 7: 1) 70 DEG C of refluxing extraction 3 hours, extracting solution is obtained sugar-cane wax at 70 DEG C of evaporates to dryness.
By confirmatory experiment, obtained sugarcane fat is weighed to obtain 257mg, and yield is 5.14%.
Be 8.98% through the total sterol content of Liebermann-Burchard colorimetric method for determining sample, after saponification plant sterol 14.42mg, the yield of plant sterol is 2.88 ‰; Sugar-cane wax 258mg, yield is 5.16%.
The method of the total sterol content of Liebermann-Burchard colorimetric method for determining sample is: the sugarcane fat that step (2) obtains, be placed in the brown measuring bottle of 10mL, add diacetyl oxide and be diluted to scale, add the vitriol oil 1, after vortex vibration 1min, leave standstill 13min, then detect its absorbance at 650nm wavelength place, and calculate its concentration according to typical curve.
Embodiment 2
(1), after Sugarcane peel. being dried pulverizing at 30 DEG C, this powder 5g 25mL alcohol is taken 30 DEG C of lixiviates 4 hours, suction filtration;
(2) gained sugarcane fat 5mL4mol/L potassium hydroxide-ethanol solution is hydrolyzed saponification 2 hours at 90 DEG C by gained filtrate after 40 DEG C of evaporates to dryness;
(3) adds 1g Repone K toward saponification liquor after hydrolysis, and with each 10mL petroleum ether extraction unsaponifiables 2 times, this extraction solution is merged evaporate to dryness and obtains plant sterol;
(4) by (1) gained filter residue 40mL normal hexane solvent (liquid ratio is 8: 1) 80 DEG C of refluxing extraction 2 hours, extracting solution is obtained sugar-cane wax at 70 DEG C of evaporates to dryness.
By confirmatory experiment, obtained sugarcane fat 202mg yield is the total sterol content of 4.05%, Liebermann-Burchard colorimetric method for determining sample is 8.53%, and obtain plant sterol 12.40mg after saponification, the yield of plant sterol is 2.48 ‰; Extraction obtains sugar-cane wax 314mg, and yield is 6.28%.
Embodiment 3
(1), after Sugarcane peel. being dried pulverizing at 30 DEG C, this powder 20g 100mL alcohol is taken 35 DEG C of lixiviates 4 hours, suction filtration;
(2) gained filtrate obtains sugarcane fat after 40 DEG C of evaporates to dryness, and gained sugarcane fat 5mL4mol/L potassium hydroxide-ethanol solution is hydrolyzed saponification 2 hours at 80 DEG C;
(3) adds 4g Repone K toward saponification liquor after hydrolysis, and with each 20mL petroleum ether extraction unsaponifiables 3 times, this extraction solution is merged evaporate to dryness and obtains plant sterol;
(4) by gained filter residue 140mL normal hexane (liquid ratio is 7: 1) in (1) 75 DEG C of refluxing extraction 2.14 hours, extracting solution is obtained sugar-cane wax at 70 DEG C of evaporates to dryness.
By confirmatory experiment, obtained sugarcane fat 774mg yield is the total sterol 8.65% of 3.87%, Liebermann-Burchard colorimetric method for determining sample, and obtain plant sterol 43.42mg after saponification, the yield of plant sterol is 2.17 ‰; Extraction obtains sugar-cane wax 1.123g, and yield is 5.62%.

Claims (1)

1. from Sugarcane peel., extract a method for plant sterol and cerosin, comprising:
(1) get Sugarcane peel., dry, pulverize obtained powder;
(2) described powder is placed in ethanol 30 ~ 35 DEG C of lixiviates 4 ~ 8 hours, lixiviate liquid ratio is 5:1, filters, and collects filtrate and filter residue;
(3) from described filtrate, extraction obtains plant sterol, utilizes normal hexane refluxing extraction to obtain cerosin from described filter residue;
The extracting method of described plant sterol is: get described filtrate, evaporate to dryness, adds the potassium hydroxide that concentration is 2 ~ 4mol/L, and saponification 2 ~ 4 hours at 80 ~ 90 DEG C, adds sherwood oil and extract, get oil phase after reacting completely, and evaporate to dryness obtains plant sterol;
In step (3), before extraction, in reaction solution, add metallic compound precipitator Repone K; During refluxing extraction, solid-liquid ratio 6 ~ 8:1; The temperature of refluxing extraction is 70 ~ 80 DEG C, and the time is 2 ~ 3h.
CN201310245316.2A 2013-06-18 2013-06-18 A kind of method extracting plant sterol and cerosin from Sugarcane peel. Active CN103319561B (en)

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CN104914180B (en) * 2015-05-13 2017-03-01 浙江大学 A kind of method measuring multi-form content of phytosterol in Caulis Sacchari sinensis
CN105273832A (en) * 2015-11-04 2016-01-27 大连工业大学 Preparation method of euphausia superba oil with low non-saponifiable matter content
CN109232701B (en) * 2017-07-10 2021-05-28 西南大学 Antitumor active monomer of sweet potato, antitumor extract of sweet potato, preparation method and application thereof
CN107603743A (en) * 2017-09-22 2018-01-19 广州聚禅现代农业研究院有限公司 A kind of extracting method of sunflower seed dregs biowax and application
CN112266403B (en) * 2020-10-28 2021-08-17 江苏科鼐生物制品有限公司 Method for extracting phytosterol by induction electric field assistance

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