CN103694207A - Method for increasing aloin extraction yield - Google Patents
Method for increasing aloin extraction yield Download PDFInfo
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- CN103694207A CN103694207A CN201310557224.8A CN201310557224A CN103694207A CN 103694207 A CN103694207 A CN 103694207A CN 201310557224 A CN201310557224 A CN 201310557224A CN 103694207 A CN103694207 A CN 103694207A
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000000605 extraction Methods 0.000 title claims abstract description 26
- AFHJQYHRLPMKHU-XXWVOBANSA-N Aloin Natural products O=C1c2c(O)cc(CO)cc2[C@H]([C@H]2[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O2)c2c1c(O)ccc2 AFHJQYHRLPMKHU-XXWVOBANSA-N 0.000 title abstract 4
- CPUHNROBVJNNPW-UHFFFAOYSA-N aloin A Natural products OC1C(O)C(O)C(CO)OC1OC1C2=CC(CO)=CC(O)=C2C(=O)C2=C(O)C=CC=C21 CPUHNROBVJNNPW-UHFFFAOYSA-N 0.000 title abstract 4
- AFHJQYHRLPMKHU-WEZNYRQKSA-N aloin B Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1[C@H]1C2=CC(CO)=CC(O)=C2C(=O)C2=C(O)C=CC=C21 AFHJQYHRLPMKHU-WEZNYRQKSA-N 0.000 title abstract 4
- AFHJQYHRLPMKHU-UHFFFAOYSA-N isobarbaloin Natural products OC1C(O)C(O)C(CO)OC1C1C2=CC(CO)=CC(O)=C2C(=O)C2=C(O)C=CC=C21 AFHJQYHRLPMKHU-UHFFFAOYSA-N 0.000 title abstract 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 39
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 34
- 235000011399 aloe vera Nutrition 0.000 claims abstract description 31
- 241001116389 Aloe Species 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000741 silica gel Substances 0.000 claims abstract description 19
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 19
- 238000010992 reflux Methods 0.000 claims abstract description 18
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 17
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 17
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 13
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000000194 supercritical-fluid extraction Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims description 24
- 239000003921 oil Substances 0.000 claims description 24
- 238000000967 suction filtration Methods 0.000 claims description 24
- AFHJQYHRLPMKHU-OSYMLPPYSA-N aloin A Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1[C@@H]1C2=CC(CO)=CC(O)=C2C(=O)C2=C(O)C=CC=C21 AFHJQYHRLPMKHU-OSYMLPPYSA-N 0.000 claims description 18
- 229940069521 aloe extract Drugs 0.000 claims description 17
- 239000012043 crude product Substances 0.000 claims description 16
- 238000010828 elution Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000007670 refining Methods 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 11
- 235000002961 Aloe barbadensis Nutrition 0.000 claims description 9
- 244000186892 Aloe vera Species 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000002425 crystallisation Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000003480 eluent Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005292 vacuum distillation Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 abstract description 6
- 241000196324 Embryophyta Species 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 238000007796 conventional method Methods 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 240000007474 Aloe arborescens Species 0.000 description 1
- 235000003011 Aloe arborescens var natalensis Nutrition 0.000 description 1
- 244000101643 Aloe ferox Species 0.000 description 1
- 235000015858 Aloe ferox Nutrition 0.000 description 1
- 241000230106 Aloe perryi Species 0.000 description 1
- 244000242092 Aloe saponaria Species 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 206010010774 Constipation Diseases 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 208000003351 Melanosis Diseases 0.000 description 1
- 230000003255 anti-acne Effects 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000002124 endocrine Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 150000004338 hydroxy anthraquinones Chemical class 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- HVGQWHMSVYODLJ-GFCCVEGCSA-N melanochrome Natural products CC1(C)Oc2cc3OC(=CC(=O)c3c(O)c2C[C@H]1O)CO HVGQWHMSVYODLJ-GFCCVEGCSA-N 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 230000000869 mutational effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000003976 plant breeding Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- CEIZFXOZIQNICU-UHFFFAOYSA-N tenuazonic acid Chemical compound CCC(C)C1NC(=O)C(C(C)=O)=C1O CEIZFXOZIQNICU-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- BPJYAXCTOHRFDQ-UHFFFAOYSA-L tetracopper;2,4,6-trioxido-1,3,5,2,4,6-trioxatriarsinane;diacetate Chemical compound [Cu+2].[Cu+2].[Cu+2].[Cu+2].CC([O-])=O.CC([O-])=O.[O-][As]1O[As]([O-])O[As]([O-])O1.[O-][As]1O[As]([O-])O[As]([O-])O1 BPJYAXCTOHRFDQ-UHFFFAOYSA-L 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D309/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
- C07D309/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
- C07D309/08—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D309/10—Oxygen atoms
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention provides a method for increasing aloin extraction yield, and belongs to the technical field of plant extraction, wherein mainly a solvent, citric acid and ammonium sulfate are added to carry out reflux extraction, a silica gel chromatographic column is adopted to carry out absorption separation, and then carbon dioxide supercritical extraction separation is performed to carry out further purification so as to achieve the increased aloin extraction yield. With the aloin extraction method, the component in the aloe raw material can be effectively precipitated, the yield of the method is increased compared with the yield of the conventional method, and the product purity is good and can achieve more than 99%.
Description
Technical field
The invention provides a kind of extracting method of aloe effective ingredient, particularly relate to the extracting method of Barbaloin A, belong to technical field of plant extraction.
Background technology
Evergreen, fleshiness herbaceous plant, leaf is large and plump, lanceolar, there is sharp tooth thorn at edge, clusters, and is a shape or is born in stem top.Inflorescence umbrella, spike or coniform, that pattern is is red, yellow or tool redness of the skin or complexion spot, six, petal, six pieces of gynoeciums.
Aloe classification mainly contains: (1) Aloe vulgaris: also claim the luxuriant aloe of drawing, U.S. aloe.The short leaf eccentric pattern of cane, is powder green, is furnished with white dot, and thick fertile juice is dense.Raceme.Be applied in the aspects such as food, medicine, cosmetics.(2) aloe sinensis: claiming again stripe aloe vera, is the mutation of storehouse aloe.Stem is short, and leaf closely clusters, and seedling leaf becomes two row leaf back adularescent spots.Originate in the medicinal and beauty treatment in Fujian, Guangdong and Guangxi Provinces, Yunnan, Sichuan, Taiwan, Hainan and island, Leizhou, tender leaf can draw raw material edible as aloe.(3) upper agricultural university leaf aloe: be the mutational variety that Department of Plant Science, Shanghai Agricultural College's plant breeding research is cultivated from Aloe vulgaris.Blade is pure white abundant without bitter taste by adularescent wax powder mesophyll, and value of exploiting and utilizing is large, and main product is in In Middle And Lower Reaches of Changjiang River.(4) Aloe arborescens var. natalensis: have another name called little wooden aloe, be regarded as very early medicinal material among the people.Originating in South Africa, is the kind most effectively of medically generally acknowledging.(5) open general aloe: claim again Aloe ferox Miller, large-scale Breeds, up to six meters, cane lignifying, leaf is large and hard, and with spine, deep green is to blue-greenish colour, by white powder.Seminal propagation is the raw material of the dry piece of the new aloe of Chinese medicine.Originate in South Africa Pu Zhou, application with medically.(6) A.saponaria: acaulescence, leafage is born in base portion, is half upright or parallel shape, eccentric pattern, its leaf juice is as suds, and the higher ornamental value of very satiny tool, has skin care effect.
Aloe can endocrine regulation, in and melanochrome, improve the synthetic function of collagen protein.Can also improve body immunity.Often eat that aloe can get rid of vivotoxin, prevents constipation, prevention of intestinal tract disease.Treatment diabetes, preventing hypertension.The all right refrigerant purging intense heat of aloe, the whole intestines effect of stomach invigorating nti-freckle, anti-acne, skin whitening, strengthen skin brightness, and skin keeps moistening and elasticity.
The activeconstituents of aloe is mainly to take Barbaloin A to be main multiple derivative in hydroxy anthraquinones category, therefore conventionally by measuring the content of Barbaloin A, assesses aloe quality, Barbaloin A have anti-inflammatory, antiviral, rush down under, the effect such as anticancer, anti-ageing, cosmetology.The extracting method of aloe mainly contains solvent-extraction process and ultrasonic extraction at present, but these traditional extracting method yields are lower, and extract purity is low, seriously polluted, is not suitable for suitability for industrialized production.
Summary of the invention
The object of this invention is to provide a kind of method that improves Barbaloin A extract yield in aloe raw material, specifically adopt following steps:
S1: get Folium Aloe 100～120 weight parts, after peeling, inner mesophyll is mashed, add normal hexane 200～240 weight parts, then add citric acid 1～3 weight part and ammonium sulfate 1～3 weight part, stir, carry out heating and refluxing extraction, return time is 1～2 hour;
S2: the feed liquid suction filtration by after refluxing extraction, obtains suction filtration liquid;
S3: to suction filtration liquid being passed in the chromatographic column that spherical reaming silica gel is housed, the composition in extracting solution is adsorbed;
S4: the chromatographic column in step S3 is carried out to wash-out, and elution speed is controlled at 2～3BV/h, elution time is 60～100 minutes;
S5: elutriant heating is concentrated into volume and becomes at 1/3 o'clock, be cooled to 2～4 ℃ of crystallizations, filtering separation, dry after, obtain Aloe extract crude product;
S6: Aloe extract crude product and No. 6 solvent oils are poured in extract carbon dioxide supercritical extraction unit according to weight ratio 1:1.5～1:2, at pressure 20～25MPa, 35 ℃～40 ℃ of temperature, under carbon dioxide flow 15～20kg/h, process 30～40min, obtain refining extract oil;
S7: the refining extract oil that step S6 is obtained, vacuum distillation drying obtains finished product.
Spherical reaming silica gel particle diameter is 200～400 orders.
Eluent preferably adopts 50%～75% (V/V) ethanolic soln.
Through lot of experiments, grope, optimum method is as follows:
S1: get Aloe Barbadensis Miller 115 weight parts, after peeling, inner mesophyll is mashed, add normal hexane 230 weight parts, then add citric acid 2.3 weight parts and ammonium sulfate 2.6 weight parts, stir, carry out heating and refluxing extraction, return time is 1 hour;
S2: the feed liquid suction filtration by after refluxing extraction, obtains suction filtration liquid;
S3: to suction filtration liquid being passed in the chromatographic column that spherical reaming silica gel is housed, the composition in extracting solution is adsorbed;
S4: the chromatographic column in step S3 is carried out to wash-out, and elution speed is controlled at 2.7BV/h, elution time is 90 minutes;
S5: elutriant heating is concentrated into volume and becomes at 1/3 o'clock, be cooled to 3 ℃ of crystallizations, filtering separation, dry after, obtain Aloe extract crude product;
S6: Aloe extract crude product and No. 6 solvent oils are poured in extract carbon dioxide supercritical extraction unit according to weight ratio 1:1.9, and at pressure 24MPa, 36 ℃ of temperature, under carbon dioxide flow 16 weight parts/h, process 38min, obtain refining extract oil;
S7: the refining extract oil that step S6 is obtained, vacuum distillation drying obtains finished product.
Spherical reaming silica gel particle diameter is 300 orders.
Eluent is to adopt 65% (V/V) ethanolic soln.
Beneficial effect
Barbaloin A extracting method provided by the invention, makes the one-tenth in aloe raw material analyze effectively, and yield is improved than traditional method, and good product purity can reach more than 99%.
Embodiment
Used silica gel of the present invention is the spherical reaming silica gel that Haiyang Chemical Plant, Qingdao produces, and particle diameter is 200-400 order, and water absorbing properties is 0.9m/ gram at least.
Embodiment 1
S1: get Aloe Barbadensis Miller 100kg, after peeling, inner mesophyll is mashed, add normal hexane 200kg, then add citric acid 1kg and ammonium sulfate 1kg, stir, carry out heating and refluxing extraction, return time is 1 hour;
S2: the feed liquid suction filtration by after refluxing extraction, obtains suction filtration liquid;
S3: to suction filtration liquid being passed in the chromatographic column that spherical reaming silica gel is housed, the composition in extracting solution is adsorbed;
S4: the chromatographic column in step S3 is carried out to wash-out, and elution speed is controlled at 2BV/h, elution time is 60 minutes;
S5: elutriant heating is concentrated into volume and becomes at 1/3 o'clock, be cooled to 2 ℃ of crystallizations, filtering separation, dry after, obtain Aloe extract crude product;
S6: Aloe extract crude product and No. 6 solvent oils are poured in extract carbon dioxide supercritical extraction unit according to weight ratio 1:1.5, and at pressure 20MPa, 35 ℃ of temperature, under carbon dioxide flow 15kg/h, process 30min, obtain refining extract oil;
S7: the refining extract oil that step S6 is obtained, vacuum distillation drying obtains finished product.
Spherical reaming silica gel particle diameter is 200～400 orders.
Eluent is to adopt 50% (V/V) ethanolic soln.
Embodiment 2
S1: get Aloe Barbadensis Miller 120kg, after peeling, inner mesophyll is mashed, add normal hexane 240kg, then add citric acid 3kg and ammonium sulfate 3kg, stir, carry out heating and refluxing extraction, return time is 2 hours;
S2: the feed liquid suction filtration by after refluxing extraction, obtains suction filtration liquid;
S3: to suction filtration liquid being passed in the chromatographic column that spherical reaming silica gel is housed, the composition in extracting solution is adsorbed;
S4: the chromatographic column in step S3 is carried out to wash-out, and elution speed is controlled at 3BV/h, elution time is 100 minutes;
S5: elutriant heating is concentrated into volume and becomes at 1/3 o'clock, be cooled to 4 ℃ of crystallizations, filtering separation, dry after, obtain Aloe extract crude product;
S6: Aloe extract crude product and No. 6 solvent oils are poured in extract carbon dioxide supercritical extraction unit according to weight ratio 1:2, and at pressure 25MPa, 40 ℃ of temperature, under carbon dioxide flow 20kg/h, process 40min, obtain refining extract oil;
S7: the refining extract oil that step S6 is obtained, vacuum distillation drying obtains finished product.
Spherical reaming silica gel particle diameter is 200～400 orders.
Eluent is to adopt 75% (V/V) ethanolic soln.
Embodiment 3
S1: get Aloe Barbadensis Miller 110kg, after peeling, inner mesophyll is mashed, add normal hexane 210kg, then add citric acid 2kg and ammonium sulfate 2kg, stir, carry out heating and refluxing extraction, return time is 1.5 hours;
S2: the feed liquid suction filtration by after refluxing extraction, obtains suction filtration liquid;
S3: to suction filtration liquid being passed in the chromatographic column that spherical reaming silica gel is housed, the composition in extracting solution is adsorbed;
S4: the chromatographic column in step S3 is carried out to wash-out, and elution speed is controlled at 2.5BV/h, elution time is 80 minutes;
S5: elutriant heating is concentrated into volume and becomes at 1/3 o'clock, be cooled to 3 ℃ of crystallizations, filtering separation, dry after, obtain Aloe extract crude product;
S6: Aloe extract crude product and No. 6 solvent oils are poured in extract carbon dioxide supercritical extraction unit according to weight ratio 1:1.7, and at pressure 22MPa, 37 ℃ of temperature, under carbon dioxide flow 18kg/h, process 35min, obtain refining extract oil;
S7: the refining extract oil that step S6 is obtained, vacuum distillation drying obtains finished product.
Spherical reaming silica gel particle diameter is 200～400 orders.
Eluent is to adopt 60% (V/V) ethanolic soln.
Embodiment 4
S1: get Aloe Barbadensis Miller 115kg, after peeling, inner mesophyll is mashed, add normal hexane 230kg, then add citric acid 2.3kg and ammonium sulfate 2.6kg, stir, carry out heating and refluxing extraction, return time is 1 hour;
S2: the feed liquid suction filtration by after refluxing extraction, obtains suction filtration liquid;
S3: to suction filtration liquid being passed in the chromatographic column that spherical reaming silica gel is housed, the composition in extracting solution is adsorbed;
S4: the chromatographic column in step S3 is carried out to wash-out, and elution speed is controlled at 2.7BV/h, elution time is 90 minutes;
S5: elutriant heating is concentrated into volume and becomes at 1/3 o'clock, be cooled to 3 ℃ of crystallizations, filtering separation, dry after, obtain Aloe extract crude product;
S6: Aloe extract crude product and No. 6 solvent oils are poured in extract carbon dioxide supercritical extraction unit according to weight ratio 1:1.9, and at pressure 24MPa, 36 ℃ of temperature, under carbon dioxide flow 16kg/h, process 38min, obtain refining extract oil;
S7: the refining extract oil that step S6 is obtained, vacuum distillation drying obtains finished product.
Spherical reaming silica gel particle diameter is 300 orders.
Eluent is to adopt 65% (V/V) ethanolic soln.
Reference examples 1
Adopt following document (Liu Yukui, Guo Yingxia, Zhao Zuolian etc., extraction separation and the assay of Barbaloin A in medicinal aloe, the medical Leader interim method of volume the 4th April the 26th in 2007 is carried out the extraction of Barbaloin A to aloe, in contrast,
Reference examples 2
Be with the difference of embodiment 1: in step S1, do not add citric acid and ammonium sulfate.
Reference examples 3
Be with the difference of embodiment 1: in step S1, do not add citric acid and ammonium sulfate.
Reference examples 4
Be with the difference of embodiment 1: in step S1, do not add citric acid and ammonium sulfate.
Performance test
The measuring method of the HPLC of Barbaloin A adopts the method in document: the preparation technology of Zhang Cuili < < Aloe extract and quality standard research > >, He'nan University, master thesis, 2008.
Embodiment and reference examples are carried out the yield of Barbaloin A and the comparison of purity.The calculation formula of yield is: finished weight/raw material weight * 100%.Test-results is as shown in table 1.
| Test parameter | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Reference examples 1 | Reference examples 2 | Reference examples 3 | Reference examples 4 |
| Yield % | 17.6% | 18.6% | 18.5% | 20.5% | 12.3% | 14.3% | 14.2% | 14.2% |
| Purity % | 99.1 | 99.2 | 99.3 | 99.6% | 96.2 | 99.1 | 98.2 | 98.4 |
As can be seen from the table, the extracting method of Barbaloin A provided by the invention, yield is higher compared with bibliographical information method, and what in document, adopt is conventional at present extracting method, final yield is about 12% left and right, and the yield of Barbaloin A provided by the invention can reach more than 17%; In addition, in the refluxing extraction of Aloe mesophyll glue, add citric acid and ammonium sulfate also to contribute to improve productive rate, if while not adding above-mentioned two kinds of salt, yield is about 14% left and right.
Barbaloin A extracting method provided by the invention, good product purity, more than 99%.Wherein, the yield of embodiment 4 and purity are optimum.
Claims (4)
1. a method that improves Barbaloin A extract yield, comprises the steps:
S1: get Folium Aloe 100～120 weight parts, after peeling, inner mesophyll is mashed, add normal hexane 200～240 weight parts, then add citric acid 1～3 weight part and ammonium sulfate 1～3 weight part, stir, carry out heating and refluxing extraction, return time is 1～2 hour;
S2: the feed liquid suction filtration by after refluxing extraction, obtains suction filtration liquid;
S3: to suction filtration liquid being passed in the chromatographic column that spherical reaming silica gel is housed, the composition in extracting solution is adsorbed;
S4: the chromatographic column in step S3 is carried out to wash-out, and elution speed is controlled at 2～3BV/h, elution time is 60～100 minutes;
S5: elutriant heating is concentrated into volume and becomes at 1/3 o'clock, be cooled to 2～4 ℃ of crystallizations, filtering separation, dry after, obtain Aloe extract crude product;
S6: Aloe extract crude product and No. 6 solvent oils are poured in extract carbon dioxide supercritical extraction unit according to weight ratio 1:1.5～1:2, at pressure 20～25MPa, 35 ℃～40 ℃ of temperature, under carbon dioxide flow 15～20kg/h, process 30～40min, obtain refining extract oil;
S7: the refining extract oil that step S6 is obtained, vacuum distillation drying obtains finished product.
2. the method for raising Barbaloin A extract yield according to claim 1, is characterized in that: described spherical reaming silica gel particle diameter is 200～400 orders.
3. the method for raising Barbaloin A extract yield according to claim 2, is characterized in that: described eluent is 50%～75% (V/V) ethanolic soln.
4. the method for raising Barbaloin A extract yield according to claim 3, is characterized in that, processing parameter is:
S1: get Aloe Barbadensis Miller 115 weight parts, after peeling, inner mesophyll is mashed, add normal hexane 230 weight parts, then add citric acid 2.3 weight parts and ammonium sulfate 2.6 weight parts, stir, carry out heating and refluxing extraction, return time is 1 hour;
S2: the feed liquid suction filtration by after refluxing extraction, obtains suction filtration liquid;
S3: to suction filtration liquid being passed in the chromatographic column that spherical reaming silica gel is housed, the composition in extracting solution is adsorbed;
S4: the chromatographic column in step S3 is carried out to wash-out, and elution speed is controlled at 2.7BV/h, elution time is 90 minutes;
S5: elutriant heating is concentrated into volume and becomes at 1/3 o'clock, be cooled to 3 ℃ of crystallizations, filtering separation, dry after, obtain Aloe extract crude product;
S6: Aloe extract crude product and No. 6 solvent oils are poured in extract carbon dioxide supercritical extraction unit according to weight ratio 1:1.9, and at pressure 24MPa, 36 ℃ of temperature, under carbon dioxide flow 16 weight parts/h, process 38min, obtain refining extract oil;
S7: the refining extract oil that step S6 is obtained, vacuum distillation drying obtains finished product; Spherical reaming silica gel particle diameter is 300 orders; Eluent is to adopt 65% (V/V) ethanolic soln.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310557224.8A CN103694207B (en) | 2013-06-30 | 2013-11-11 | Method for increasing aloin extraction yield |
Applications Claiming Priority (3)
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104402851A (en) * | 2014-09-30 | 2015-03-11 | 江苏奇力康皮肤药业有限公司 | Method for extracting barbaloin used for cosmetic |
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Non-Patent Citations (2)
| Title |
|---|
| 卢智: "《超临界流体萃取芦荟苷的研究》", 《食品工业》 * |
| 孙婉华等: "《芦荟汁中芦荟苷的稳定化技术研究》", 《热带农业科学》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402851A (en) * | 2014-09-30 | 2015-03-11 | 江苏奇力康皮肤药业有限公司 | Method for extracting barbaloin used for cosmetic |
| CN104402851B (en) * | 2014-09-30 | 2016-08-24 | 江苏奇力康皮肤药业有限公司 | A kind of extracting method of the barbaloin for cosmetics |
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