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 PDFInfo
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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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- 240000000111 Saccharum officinarum Species 0.000 title claims abstract description 53
- 235000007201 Saccharum officinarum Nutrition 0.000 title claims abstract description 53
- 235000002378 plant sterols Nutrition 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000706 filtrate Substances 0.000 claims abstract description 15
- 238000010992 reflux Methods 0.000 claims abstract description 13
- 239000000284 extract Substances 0.000 claims abstract description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- 238000007127 saponification reaction Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 10
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 229910000765 intermetallic Inorganic materials 0.000 claims description 3
- 239000012716 precipitator Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000002904 solvent Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 231100000957 no side effect Toxicity 0.000 abstract description 2
- 239000001993 wax Substances 0.000 description 17
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 229930182558 Sterol Natural products 0.000 description 6
- 229960004756 ethanol Drugs 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 235000019198 oils Nutrition 0.000 description 6
- 150000003432 sterols Chemical class 0.000 description 6
- 235000003702 sterols Nutrition 0.000 description 6
- LGJMUZUPVCAVPU-UHFFFAOYSA-N beta-Sitostanol Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(C)CCC(CC)C(C)C)C1(C)CC2 LGJMUZUPVCAVPU-UHFFFAOYSA-N 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 5
- OILXMJHPFNGGTO-UHFFFAOYSA-N (22E)-(24xi)-24-methylcholesta-5,22-dien-3beta-ol Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)C=CC(C)C(C)C)C1(C)CC2 OILXMJHPFNGGTO-UHFFFAOYSA-N 0.000 description 4
- OQMZNAMGEHIHNN-UHFFFAOYSA-N 7-Dehydrostigmasterol Natural products C1C(O)CCC2(C)C(CCC3(C(C(C)C=CC(CC)C(C)C)CCC33)C)C3=CC=C21 OQMZNAMGEHIHNN-UHFFFAOYSA-N 0.000 description 4
- HZYXFRGVBOPPNZ-UHFFFAOYSA-N UNPD88870 Natural products C1C=C2CC(O)CCC2(C)C2C1C1CCC(C(C)=CCC(CC)C(C)C)C1(C)CC2 HZYXFRGVBOPPNZ-UHFFFAOYSA-N 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 4
- 238000004737 colorimetric analysis Methods 0.000 description 4
- CNNRPFQICPFDPO-UHFFFAOYSA-N octacosan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCCO CNNRPFQICPFDPO-UHFFFAOYSA-N 0.000 description 4
- HCXVJBMSMIARIN-PHZDYDNGSA-N stigmasterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)/C=C/[C@@H](CC)C(C)C)[C@@]1(C)CC2 HCXVJBMSMIARIN-PHZDYDNGSA-N 0.000 description 4
- 235000016831 stigmasterol Nutrition 0.000 description 4
- 229940032091 stigmasterol Drugs 0.000 description 4
- BFDNMXAIBMJLBB-UHFFFAOYSA-N stigmasterol Natural products CCC(C=CC(C)C1CCCC2C3CC=C4CC(O)CCC4(C)C3CCC12C)C(C)C BFDNMXAIBMJLBB-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 235000013311 vegetables Nutrition 0.000 description 3
- 229960002666 1-octacosanol Drugs 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 235000012000 cholesterol Nutrition 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000004332 deodorization Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- YLLIGHVCTUPGEH-UHFFFAOYSA-M potassium;ethanol;hydroxide Chemical compound [OH-].[K+].CCO YLLIGHVCTUPGEH-UHFFFAOYSA-M 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940076810 beta sitosterol Drugs 0.000 description 1
- NJKOMDUNNDKEAI-UHFFFAOYSA-N beta-sitosterol Natural products CCC(CCC(C)C1CCC2(C)C3CC=C4CC(O)CCC4C3CCC12C)C(C)C NJKOMDUNNDKEAI-UHFFFAOYSA-N 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 210000002615 epidermis Anatomy 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 208000019622 heart disease Diseases 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 235000014571 nuts Nutrition 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 239000012165 plant wax Substances 0.000 description 1
- 229960001109 policosanol Drugs 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- KZJWDPNRJALLNS-VJSFXXLFSA-N sitosterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CC[C@@H](CC)C(C)C)[C@@]1(C)CC2 KZJWDPNRJALLNS-VJSFXXLFSA-N 0.000 description 1
- 229950005143 sitosterol Drugs 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 230000003637 steroidlike Effects 0.000 description 1
- 229960004793 sucrose Drugs 0.000 description 1
- -1 tetracol phenixin Substances 0.000 description 1
- 230000005760 tumorsuppression Effects 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 239000012178 vegetable wax Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
Landscapes
- Steroid Compounds (AREA)
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
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.
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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 |
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