CN112957764A - Method for extracting asiaticoside-rich composition from centella asiatica - Google Patents
Method for extracting asiaticoside-rich composition from centella asiatica Download PDFInfo
- Publication number
- CN112957764A CN112957764A CN202110135003.6A CN202110135003A CN112957764A CN 112957764 A CN112957764 A CN 112957764A CN 202110135003 A CN202110135003 A CN 202110135003A CN 112957764 A CN112957764 A CN 112957764A
- Authority
- CN
- China
- Prior art keywords
- sff
- extraction
- tank
- centella asiatica
- spe
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 244000146462 Centella asiatica Species 0.000 title claims abstract description 89
- 235000004032 Centella asiatica Nutrition 0.000 title claims abstract description 89
- QCYLIQBVLZBPNK-UHFFFAOYSA-N asiaticoside A Natural products O1C(C(=O)C(C)C)=CC(C)C(C2(C(OC(C)=O)CC34C5)C)C1CC2(C)C3CCC(C1(C)C)C45CCC1OC1OCC(O)C(O)C1O QCYLIQBVLZBPNK-UHFFFAOYSA-N 0.000 title claims abstract description 54
- WYQVAPGDARQUBT-FGWHUCSPSA-N Madecassol Chemical compound O([C@@H]1[C@@H](CO)O[C@H]([C@@H]([C@H]1O)O)OC[C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)OC(=O)[C@]12CC[C@H]([C@@H]([C@H]1C=1[C@@]([C@@]3(CC[C@H]4[C@](C)(CO)[C@@H](O)[C@H](O)C[C@]4(C)[C@H]3CC=1)C)(C)CC2)C)C)[C@@H]1O[C@@H](C)[C@H](O)[C@@H](O)[C@H]1O WYQVAPGDARQUBT-FGWHUCSPSA-N 0.000 title claims abstract description 53
- WYQVAPGDARQUBT-XCWYDTOWSA-N asiaticoside Natural products O=C(O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO[C@H]2[C@H](O)[C@H](O)[C@H](O[C@H]3[C@H](O)[C@H](O)[C@@H](O)[C@H](C)O3)[C@@H](CO)O2)O1)[C@@]12[C@@H]([C@@H](C)[C@H](C)CC1)C=1[C@](C)([C@@]3(C)[C@@H]([C@@]4(C)[C@H]([C@@](CO)(C)[C@@H](O)[C@H](O)C4)CC3)CC=1)CC2 WYQVAPGDARQUBT-XCWYDTOWSA-N 0.000 title claims abstract description 53
- 229940022757 asiaticoside Drugs 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000000203 mixture Substances 0.000 title claims abstract description 44
- 238000000605 extraction Methods 0.000 claims abstract description 109
- 238000005194 fractionation Methods 0.000 claims abstract description 70
- 239000000284 extract Substances 0.000 claims abstract description 31
- 229940059958 centella asiatica extract Drugs 0.000 claims abstract description 27
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 100
- 239000001294 propane Substances 0.000 claims description 50
- 239000012530 fluid Substances 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000000926 separation method Methods 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 238000002137 ultrasound extraction Methods 0.000 claims description 5
- 238000000658 coextraction Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 125000003158 alcohol group Chemical group 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229930014626 natural product Natural products 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 22
- 208000033962 Fontaine progeroid syndrome Diseases 0.000 description 22
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 22
- 238000001228 spectrum Methods 0.000 description 20
- 238000003860 storage Methods 0.000 description 19
- 229910002092 carbon dioxide Inorganic materials 0.000 description 12
- 239000001569 carbon dioxide Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 8
- 239000007788 liquid Substances 0.000 description 5
- 210000003491 skin Anatomy 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 238000003809 water extraction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 102000008186 Collagen Human genes 0.000 description 2
- 108010035532 Collagen Proteins 0.000 description 2
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 description 2
- 208000028990 Skin injury Diseases 0.000 description 2
- LBGFKBYMNRAMFC-PYSQTNCISA-N asiatic acid Natural products C[C@@H]1CC[C@@]2(CC[C@]3(C)C(=CC[C@@H]4[C@@]5(C)C[C@@H](O)[C@H](O)[C@@](C)(CO)[C@@H]5CC[C@@]34C)[C@]2(C)[C@H]1C)C(=O)O LBGFKBYMNRAMFC-PYSQTNCISA-N 0.000 description 2
- JXSVIVRDWWRQRT-UYDOISQJSA-N asiatic acid Chemical compound C1[C@@H](O)[C@H](O)[C@@](C)(CO)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CC[C@@H](C)[C@H](C)[C@H]5C4=CC[C@@H]3[C@]21C JXSVIVRDWWRQRT-UYDOISQJSA-N 0.000 description 2
- 229940011658 asiatic acid Drugs 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229920001436 collagen Polymers 0.000 description 2
- 210000004207 dermis Anatomy 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- CLXOLTFMHAXJST-UHFFFAOYSA-N esculentic acid Natural products C12CC=C3C4CC(C)(C(O)=O)CCC4(C(O)=O)CCC3(C)C1(C)CCC1C2(C)CCC(O)C1(CO)C CLXOLTFMHAXJST-UHFFFAOYSA-N 0.000 description 2
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 2
- IYRMWMYZSQPJKC-UHFFFAOYSA-N kaempferol Chemical compound C1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 IYRMWMYZSQPJKC-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 241000208173 Apiaceae Species 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- 241000180579 Arca Species 0.000 description 1
- UBSCDKPKWHYZNX-UHFFFAOYSA-N Demethoxycapillarisin Natural products C1=CC(O)=CC=C1OC1=CC(=O)C2=C(O)C=C(O)C=C2O1 UBSCDKPKWHYZNX-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241001013934 Erigeron breviscapus Species 0.000 description 1
- 102000009123 Fibrin Human genes 0.000 description 1
- 108010073385 Fibrin Proteins 0.000 description 1
- BWGVNKXGVNDBDI-UHFFFAOYSA-N Fibrin monomer Chemical compound CNC(=O)CNC(=O)CN BWGVNKXGVNDBDI-UHFFFAOYSA-N 0.000 description 1
- BNMGUJRJUUDLHW-HLUHVYOBSA-N Madecassoside Natural products C[C@@H]1CC[C@@]2(CC[C@]3(C)C(=CC[C@@H]4[C@@]5(C)C[C@@H](O)[C@H](O)[C@@](C)(CO)[C@@H]5[C@H](O)C[C@@]34C)[C@@H]2[C@H]1C)C(=O)O[C@@H]6O[C@H](CO[C@@H]7O[C@H](CO)[C@@H](O[C@@H]8O[C@H](C)[C@H](O)[C@@H](O)[C@H]8O)[C@H](O)[C@H]7O)[C@@H](O)[C@H](O)[C@H]6O BNMGUJRJUUDLHW-HLUHVYOBSA-N 0.000 description 1
- BNMGUJRJUUDLHW-HCZMHFOYSA-N Madecassoside Chemical compound O([C@@H]1[C@@H](CO)O[C@H]([C@@H]([C@H]1O)O)OC[C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)OC(=O)[C@]12CC[C@H]([C@@H]([C@H]1C=1[C@@]([C@@]3(C[C@@H](O)[C@H]4[C@](C)(CO)[C@@H](O)[C@H](O)C[C@]4(C)[C@H]3CC=1)C)(C)CC2)C)C)[C@@H]1O[C@@H](C)[C@H](O)[C@@H](O)[C@H]1O BNMGUJRJUUDLHW-HCZMHFOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 description 1
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 description 1
- 241001506047 Tremella Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 210000002615 epidermis Anatomy 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229950003499 fibrin Drugs 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 238000010262 high-speed countercurrent chromatography Methods 0.000 description 1
- 235000008777 kaempferol Nutrition 0.000 description 1
- 229940090813 madecassoside Drugs 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 description 1
- LRTFPLFDLJYEKT-UHFFFAOYSA-N para-isopropylaniline Chemical compound CC(C)C1=CC=C(N)C=C1 LRTFPLFDLJYEKT-UHFFFAOYSA-N 0.000 description 1
- 235000005875 quercetin Nutrition 0.000 description 1
- 229960001285 quercetin Drugs 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000033764 rhythmic process Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000010898 silica gel chromatography Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 230000017423 tissue regeneration Effects 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
Abstract
The invention discloses a method for extracting a composition rich in asiaticoside from centella asiatica, and relates to the technical field of natural product extraction. The method comprises the following steps: s1, cleaning and drying the centella asiatica, and adding an extraction solvent for extraction to obtain centella asiatica extract; and S2, carrying out supercritical fractionation on the centella asiatica extract. The method for extracting the composition rich in asiaticoside from the centella asiatica roots, provided by the invention, has the advantages that the centella asiatica root extract is further fractionated by adopting a supercritical fractionation mode on the basis of obtaining the centella asiatica root extract by the original extraction mode, the extraction rate is improved, and the supercritical fractionation mode is simpler than the traditional methods such as heavy crystallization and the like, the production capacity is high, the cost is lower, and the industrial value is higher.
Description
Technical Field
The invention relates to the technical field of natural product extraction, in particular to a method for extracting a composition rich in asiaticoside from centella asiatica.
Background
Centella asiatica, arca paniculata, erigeron breviscapus, tremella aurantii, ramose palustre and umbelliferae herbaceous plants. The centella asiatica contains chemical components including asiaticoside, madecassoside, ginseng cumidine, asiatic acid, asiatic sugar, kaempferol, quercetin, etc. In recent years, researches show that centella asiatica can tighten the connecting part of epidermis and dermis, can soften the skin, is beneficial to solving the skin relaxation phenomenon (especially for postpartum mothers), and enables the skin to be smooth and elastic; the collagen in the dermis is promoted to be formed, the fibrin is regenerated and is connected again, and the skin achieves the effects of tightening and smoothing. Can also help the injured tissue to heal and compact the skin.
The centella asiatica extract can effectively promote skin injury and local collagen anabolism, and has an important effect on the aspect of tissue repair after skin injury.
The method for separating asiaticoside from centella asiatica mainly comprises silica gel column chromatography, macroporous resin adsorption, aqueous two-phase extraction, ultrafiltration membrane separation, and supercritical CO2Fluid extraction, high-speed counter-current chromatography, etc., which all have certain disadvantages and are not suitable for industrial production. The main problems are as follows: the process is complex, the material consumption is too large, the yield is low, and the treatment capacity is not large.
For example, CN102532244A discloses a method for preparing high-purity asiaticoside, which is obtained by separation with solvent extraction method, and has complicated steps, high consumption, and is not suitable for industrial production.
CN106946971A discloses a process for extracting asiatic acid from centella asiatica, which is complex in process, small in treatment amount and high in cost through a method of multiple decolorization and recrystallization.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for extracting a composition rich in asiaticoside from centella asiatica by using a subcritical propane fluid extraction method.
Another object of the present invention is to provide a method for extracting a composition rich in asiaticoside from centella asiatica by using a subcritical propane fluid extraction method and a supercritical fractionation method.
In order to solve the above problems, the present invention proposes the following technical solutions:
a method for extracting a composition rich in asiaticoside from centella asiatica comprises the following steps:
s1, cleaning and drying the centella asiatica, and adding an extraction solvent for extraction to obtain centella asiatica extract;
s2, performing supercritical fractionation on the centella asiatica extract, wherein the supercritical fractionation hardware at least comprises an SFF extraction tank, a first SFF fractionation tank and a second SFF fractionation tank;
the supercritical fractionation conditions are as follows: the pressure of the SFF extraction tank is 75-300 bar, and the temperature is 32-100 ℃; the pressure of the first SFF fractionating tank is 70-150 bar, the temperature is 32-100 ℃, the pressure of the second SFF fractionating tank is 40-200 bar, the temperature is 32-100 ℃, and CO is2The flow rate is adjusted according to the capacity.
Understandably, the Supercritical Fluid fractionation technique (hereinafter SFF) wherein the SFF hardware comprises at least an SFF extraction tank, a first SFF fractionation tank and a second SFF fractionation tank, see fig. 11.
The further technical scheme is that the extraction solvent is water, and the S1 extraction step is as follows:
cleaning and drying centella asiatica, adding 2-4 times of water by mass, and extracting at 90-110 ℃ for 0.5-1.5h to obtain an extract;
cooling the extract to room temperature, concentrating and filtering to obtain a concentrated solution;
in order to improve the fractionation efficiency, 5-10 times volume of alcohol is added into the concentrated solution for dilution to obtain a centella asiatica extract, and the centella asiatica extract is introduced into an SFF extraction tank for supercritical fractionation.
The further technical scheme is that the extraction solvent is alcohol, and the S1 extraction step is as follows:
cleaning and drying centella asiatica, adding 2-4 times of alcohol by mass, and performing ultrasonic extraction for 0.5-1.5h to obtain an extract;
and filtering the extract, and concentrating to 1/6-1/3 of the volume of the alcohol to obtain the centella asiatica extract.
More preferably, the method for extracting the composition rich in asiaticoside from centella asiatica is a method for extracting the composition rich in asiaticoside from centella asiatica by using a subcritical propane fluid extraction method and a supercritical fractionation method (SPE + SFF technology). The method comprises the following specific steps:
cleaning and drying centella asiatica, and crushing to obtain centella asiatica root powder;
pouring the centella asiatica root powder into an SPE extraction tank of a subcritical propane fluid extraction device for subcritical propane fluid extraction;
introducing the extraction fluid into an SPE separation tank;
removing propane in the SPE separation tank to obtain a centella asiatica extract;
and carrying out supercritical fractionation on the centella asiatica extract.
Wherein, the subcritical propane fluid extraction conditions are as follows: the pressure of the SPE extraction tank is 0.2-0.5 Mpa, and the temperature is 30-60 ℃.
The supercritical fractionation conditions are as follows: the pressure of the SFF extraction tank is 75-300 bar, and the temperature is 32-100 ℃; the pressure of the first SFF fractionating tank is 70-150 bar, the temperature is 32-100 ℃, the pressure of the second SFF fractionating tank is 40-200 bar, the temperature is 32-100 ℃, and CO is2The flow rate is adjusted according to the capacity.
Preferably, the preferred conditions for the supercritical fractionation are: the pressure of the SFF extraction tank is 85-200 bar, and the temperature is 32-80 ℃; the pressure of the first SFF fractionating tank is 70-120 bar, the temperature is 32-80 ℃, the pressure of the second SFF fractionating tank is 40-100 bar, and the temperature is 32-80 ℃.
More preferably, the more preferable conditions for supercritical fractionation are: the pressure of the SFF extraction tank is 90-210 bar, and the temperature is 40-80 ℃; the pressure of the first SFF fractionating tank is 74-120 bar, and the temperature is 40-80 ℃; the pressure of the second SFF fractionating tank is 44-100 bar, and the temperature is 40-80 ℃.
The grinding operation of the centella asiatica is only to improve the extraction effect and the extraction rate, the particle size of the centella asiatica powder is too large, the extraction effect is poor, and generally the particle size is preferably 0.5-5 mm.
In order to improve the fractionation effect, in the step of extracting the subcritical propane fluid, alcohol with the volume of 5-10% of that of the extraction solvent is added for co-extraction.
The Subcritical Propane fluid Extraction technology (hereinafter referred to as SPE), wherein the pressure of the SPE Extraction tank is preferably 0.2-0.5 MPa, more preferably 0.3-0.45 MPa, and even more preferably 0.4 MPa; the temperature of the SPE extraction tank is 30-60 ℃, preferably 40-55 ℃, and more preferably 50 ℃; the pressure of the SPE separation tank is not lower than that of the propane storage tank, generally 8-10 bar; the SPE separation tank temperature is preferably higher than the boiling point of propane, generally a temperature above room temperature, preferably 45-60 deg.C, and the propane flow rate depends on the productivity of the asiaticoside-rich composition, generally 0.7-1 times the volume of the SPE extraction tank.
With further reference to FIG. 11, the SPE extraction apparatus hardware contains at least a SPE extraction tank, a SPE separation tank, and a propane storage tank.
In order to improve the fractionation efficiency, the subcritical propane fluid extraction step is performed, and the subcritical propane fluid extraction step further comprises adding alcohol with the volume of 5-10% of that of the extraction solvent for co-extraction.
In one suitable example, the SPE technique and SFF technique described above may be operated separately and independently, e.g., see fig. 11; however, it is preferable that the SPE technique and the SFF technique are combined to form an integrated operation, for example, see FIGS. 12a to 12c, and 13a to 13 d; FIGS. 12a to 12c show a batch-type integrated operation mode; fig. 13a to 13d show a continuous integrated operation mode, and a continuous integrated operation mode (fig. 13a to 13d) is more preferable.
The following detailed description describes the apparatus according to the invention for extracting a composition rich in asiaticoside from centella asiatica by means of a subcritical propane fluid extraction process and a supercritical fractionation process (SPE + SFF technique), the apparatus comprising:
an SPE module comprising a propane tank (110), and an SPE extraction tank (120);
at least one first common slot (210);
an SFF assembly comprising a first SFF fractionation tank (330), a second SFF fractionation tank (340) connected in series; and
a controller assembly comprising a first shared controller (A21), a first SFF controller (A31), and a second SFF controller (A32); wherein the first shared controller (A21) is located between the SPE extraction tank and a first shared tank body (210); the first SFF controller (A31) located between the first shared controller (A21) and the carbon dioxide storage tank (310); the second SFF controller (A32) located between the first shared tank (210) and the first SFF fractionation tank (330);
when SPE operation is executed, the propane storage tank (110), the SPE extraction tank (120), the first sharing controller (A21) and the first sharing tank body (210) are in a conducting state to form an SPE device so as to execute the SPE operation; the first SFF controller (A31) and the second SFF controller (A32) are in a closed state;
when an SFF operation is performed, the carbon dioxide storage tank (310), the first SFF controller (a31), the first shared controller (a21), the first shared tank body (210), the second SFF controller (a32), the first SFF fractionating tank (330), and the second SFF fractionating tank (340) are sequentially connected in an on state to constitute an SFF device to perform an SFF operation; and a closed circuit state is established between the first shared controller (A21) and the SPE extraction tank (120).
The further technical solution is that, please continue to refer to fig. 12 a-12 c, 13 a-13 d, the present invention provides a device for extracting a composition rich in asiaticoside from centella asiatica, which comprises:
an SPE module, said SPE module comprising a propane storage tank (110), SPE extraction tank (120);
a shared slot assembly comprising a first shared slot (210) and a second shared slot (220);
an SFF assembly comprising a first SFF fractionation tank (330), a second SFF fractionation tank (340) connected in series; and
a controller assembly comprising an SPE controller (A11), a first shared controller (A21), a second shared controller (A22), a first SFF controller (A31), and a second SFF controller (A32); wherein the SPE controller (A11) is respectively connected with the SPE extraction tank (120), the first shared controller (A21) and the second shared controller (A22); the first sharing controller (A21) is respectively connected with the SPE controller (A11), the first sharing slot body (210) and the first SFF controller (A31); the second sharing controller (A22) is respectively connected with the SPE controller (A11), the second sharing slot body (220) and the first SFF controller (A31); the first SFF controller (A31) is respectively connected with the first shared controller (A21), the second shared controller (A22) and the carbon dioxide storage tank; the second SFF controller (A32) is respectively connected with the first shared groove body (210), the second shared groove body (220) and the first SFF fractionating groove (330);
the controller assembly can be continuously and automatically switched into two operation modes
(1) A closed state is formed between the SPE controller (A11) and the second sharing controller (A22), a closed state is formed between the first SFF controller (A31) and the first sharing controller (A21), and a closed state is formed between the second SFF controller (A32) and the first sharing slot body (210); the propane storage tank (110), the SPE extraction tank (120), the SPE controller (A11), the first sharing controller (A21) and the first sharing tank body (210) are sequentially connected to form an independent SPE device; meanwhile, a carbon dioxide storage tank (310), a first SFF controller (A31), a second shared controller (A22), a second shared tank body (220), a second SFF controller (A32), a first SFF fractionating tank (330) and a second SFF fractionating tank (340) are sequentially connected to form an independent SFF device;
(2) a closed state is formed between the SPE controller (A11) and the first shared controller (A21), a closed state is formed between the first SFF controller (A31) and the second shared controller (A22), and a closed state is formed between the second SFF controller (A32) and the second shared slot body (220); the propane storage tank (110), the SPE extraction tank (120), the SPE controller (A11), the second shared controller (A22) and the second shared tank body (220) are sequentially connected to form an independent SPE device; meanwhile, a carbon dioxide storage tank (310), a first SFF controller (A31), a first shared controller (A21), a first shared tank body (210), a second SFF controller (A32), a first SFF fractionating tank (330) and a second SFF fractionating tank (340) are sequentially connected to form an independent SFF device.
Compared with the prior art, the invention can achieve the following technical effects:
(1) the method for extracting the composition rich in asiaticoside from the centella asiatica provided by the invention is characterized in that the centella asiatica extract is further fractionated by adopting a supercritical fractionation mode on the basis of obtaining the centella asiatica extract by the original extraction mode, so that the extraction rate is improved, and the supercritical fractionation mode is simpler than the traditional methods such as heavy crystallization and the like, and has the advantages of high yield, lower cost and higher industrial value.
(2) The applicant finds that the invention simultaneously adopts a subcritical propane fluid extraction method to extract centella asiatica roots, and then adopts a supercritical fractionation method to carry out supercritical fractionation on the extract so as to extract the composition rich in asiaticoside; the technical effect of using the subcritical propane fluid extraction method is as follows: (1) the centella asiatica is extracted by subcritical propane fluid, and centella asiatica extract containing asiaticoside can be obtained at high efficiency; (2) extracting centella asiatica with subcritical propane fluid to obtain centella asiatica extract; (3) under specific temperature and pressure, the centella asiatica is extracted by subcritical propane fluid, so that propane can be recovered, and the purposes of low cost and environmental protection are achieved; the technical effect of adopting the supercritical fractionation method is as follows: the centella asiatica extract containing asiaticoside is further fractionated by a supercritical fractionation method to obtain the composition rich in asiaticoside, is efficient and convenient, and is suitable for industrial production.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is the GCMS spectrum of the asiaticoside composition obtained by extracting centella asiatica with water in example 1.
FIG. 2 is a GCMS spectrum of the asiaticoside composition obtained in example 1 by water extraction of centella asiatica followed by supercritical fractionation using the first SFF fractionation tank.
FIG. 3 is a GCMS spectrum of the asiaticoside composition obtained by water extraction of centella asiatica in example 1 and then using supercritical fractionation technology, a second SFF fractionation tank.
FIG. 4 is the GCMS spectrum of the asiaticoside composition obtained from the bottom of the SFF extraction tank in example 1 by extracting centella asiatica with water and then using supercritical fractionation technology.
FIG. 5 is the GCMS spectrum of the asiaticoside composition obtained by extracting centella asiatica with wine in example 2.
FIG. 6 is the GCMS spectrum of the asiaticoside composition obtained by the alcohol extraction of centella asiatica in example 2 and the supercritical fractionation in the first SFF fractionation tank.
FIG. 7 is the GCMS spectrum of the asiaticoside composition obtained by the extraction of centella asiatica with wine and the supercritical fractionation technique at the bottom of the SFF extraction tank in example 2.
FIG. 8 is the GCMS spectrum of the asiaticoside composition contained in the extract of centella asiatica obtained by the SPE extraction of centella asiatica in example 3.
FIG. 9 is a GCMS spectrum of the asiaticoside composition obtained in the SPE + SFF extraction of centella asiatica in example 3, the first SFF fractionation tank.
FIG. 10 is a GCMS spectrum of the asiaticoside composition obtained in the SPE + SFF extraction of centella asiatica in example 3 and the second SFF fractionation tank.
FIG. 11 is a schematic view of an apparatus for extracting a composition rich in asiaticoside from centella asiatica according to an embodiment of the present invention.
FIGS. 12 a-12 c are schematic views of an apparatus and an operation method for extracting a composition rich in asiaticoside from centella asiatica according to another embodiment of the present invention.
FIGS. 13 a-13 d are schematic views of an apparatus and an operation method for extracting a composition rich in asiaticoside from centella asiatica according to another embodiment of the present invention.
Reference numerals
Detailed Description
The technical solutions in the embodiments will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, wherein like reference numerals represent like elements in the drawings. It is apparent that the embodiments to be described below are only a part of the embodiments of the present invention, and not all of them. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
FIG. 11 shows a schematic diagram of an apparatus for extracting a composition rich in asiaticoside from centella asiatica according to an embodiment of the present invention, which includes SPE and SFF devices. Wherein the SPE part comprises a propane storage tank 110, an SPE extraction tank 120 and an SPE separation tank 130; an SFF part carbon dioxide-containing storage tank 310, an SFF extraction tank 320, a first SFF fractionating tank 330 and a second SFF fractionating tank 340; while SPE devices and SFF devices each operate independently. In fig. 11, the SPE extraction tank 120 is used for placing the centella asiatica powder (particles) to be extracted and performing SPE operation after introducing the subcritical propane fluid; the extracted centella asiatica root extract forms a propane (subcritical fluid) solution containing asiaticoside, the propane solution enters the SPE separation tank 130, the centella asiatica root extract containing the asiaticoside is obtained after the propane is discharged (recovered), and the SPE operation is finished. The centella asiatica extract in the SPE separation tank 130 is transferred to the SFF extraction tank 320, and after introducing the supercritical carbon dioxide fluid, SFF operation is performed, and the first SFF fractionation tank 330 can obtain the composition rich in asiaticoside.
A schematic diagram of a device for extracting a asiaticoside-rich composition from centella asiatica according to another embodiment of the present invention is shown in fig. 12a, which is a combination device of SPE and SFF, wherein the SPE separation tank and the SFF extraction tank share the same tank, i.e., the first shared tank 210 in fig. 12 a; and a first sharing controller A21, a first SFF controller A31 and a second SFF controller A32 are additionally arranged, and the functions of the first sharing controller A21, the first SFF controller A31 and the second SFF controller A32 are as follows: when SPE operation is performed, as shown in fig. 12b, the first shared controller a21 is turned on, so SPE can be implemented smoothly (solid line part in fig. 12 b), the first SFF controller a31 and the second SFF controller a32 are closed, SFF is not performed (dotted line part in fig. 12 b), that is, only SPE operation is performed; when the SFF operation is performed, as shown in fig. 12c, the first SFF controller a31 and the second SFF controller a32 are connected, so the SFF operation can be smoothly performed (solid line portion in fig. 12 c), the first shared controller a21 is closed, the SPE is not performed (dotted line portion in fig. 12 c), that is, only the SFF operation is performed. The device for extracting the asiaticoside-rich composition from centella asiatica provided by this embodiment can save a tank (SPE separation tank or SFF extraction tank), and can omit the operation procedure of "moving the centella asiatica extract in the SPE separation tank 130 into the SFF extraction tank 320" provided by the embodiment shown in fig. 11.
Fig. 13a is a schematic view of an apparatus for extracting a composition rich in asiaticoside from centella asiatica according to another embodiment of the present invention, and with respect to fig. 12a, the apparatus of this embodiment is additionally provided with a second shared tank 220, an SPE controller a11 and a second shared controller a22, so as to achieve an automatic/continuous production mode, and during the continuous operation (fig. 13c and 13d), there is no idle apparatus, so that the production rhythm is compact. The operation mechanism is introduced as follows:
(1) as shown in fig. 13b, the second shared controller a22, the first SFF controller a31, and the second SFF controller a32 are in a closed state (dashed line in fig. 13 b), the first shared controller a21 is in an open state, and the SPE controller a11 selects a direction (solid line in fig. 13 b) to the first shared controller a 21/first shared tank 210, and only performs SPE operation to perform SPE operation on the 1st batch of rangium wilfordii root powder to obtain the 1st batch of rangium wilfordii root extract as a raw material for performing the SFF operation;
(2) as shown in fig. 13c, SPE controller a11 is selectively led to second shared controller a 22/second shared trough body 220 (solid line part in fig. 13 c), first SFF controller a31 is selectively led to first shared controller a 21/first shared trough body 210 (solid line part in fig. 13 c), and second SFF controller a32 and second shared trough body 220 are in a closed state (dotted line part in fig. 13 c), that is, carbon dioxide storage tank 310, first SFF controller a 31/first shared controller a21, first shared trough body 210, second SFF controller a32, first SFF fractionating trough 330, and second SFF fractionating trough 340 constitute a set of independent SFF devices in sequence, so as to perform supercritical fractionation on the 1st rang of rang extract in (1); meanwhile, the propane storage tank 110, the SPE extraction tank 120, the SPE controller a11, the second shared controller a22, and the second shared tank 220 sequentially form a group of independent SPE devices for performing SPE operation on the 2nd batch of centella asiatica root powder to obtain the 2nd batch of centella asiatica root extract as a next batch of raw material for SFF operation;
(3) as shown in fig. 13d, SPE controller a11 is selectively open to the first shared controller a 21/the first shared tank 210 (solid line part in fig. 13d), the first SFF controller a31 is selectively open to the second shared controller a 22/the second shared tank 220 (solid line part in fig. 13d), and the second SFF controller a32 and the first shared tank 210 are in a closed state (dotted line part in fig. 13d), that is, the carbon dioxide storage tank 310, the first SFF controller 31/the second shared controller 22, the second shared tank 220, the second SFF controller 32, the first SFF fractionating tank 330, and the second SFF fractionating tank 340 sequentially form a set of independent SFF devices for performing supercritical fractionation on the 2nd batch of the raney public root extract in (2); meanwhile, the propane storage tank 110, the SPE extraction tank 120, the SPE controller a11, the first shared controller a21, and the first shared tank 210 sequentially form a group of independent SPE devices for performing SPE operation on the 3 rd batch of centella asiatica root powder to obtain the 3 rd batch of centella asiatica root extract as a raw material for performing the next batch of SFF operation;
then, the operations (2), (3), (2) and (3) … are executed alternately, wherein the operation (2) is executed the nth time: SFF carries out supercritical fractionation operation on the 2n-1 batch of centella asiatica extracts; SPE performs SPE operation on the 2 nth batch of the centella asiatica root powder to obtain 2 nth batch of centella asiatica root extract; the operation of executing (3) n times is: SFF carries out supercritical fractionation operation on the 2 nth batch of centella asiatica extracts; SPE performs SPE operation on the 2n +1 batch of the centella asiatica root powder to obtain the 2n +1 batch of the centella asiatica root extract.
It is understood that in other embodiments, the SPE device is preferably provided with a propane recovery device, the SFF device is preferably provided with a carbon dioxide recovery system, and the SPE and SFF devices are preferably provided with a check valve, a booster pump, a preheater, a discharge valve, a control valve, etc., which are well known in the prior art of SPE and SFF.
Specific examples are detailed below:
example 1
The preparation method of the centella asiatica water extraction (CW) comprises the following steps:
a. firstly, cleaning and drying the centella asiatica.
b. The 1000 g of the weighing scale is put into the pan.
c. 3000cc of water was added to the pan.
d. Boiling the pot containing centella asiatica and water, and then rolling for 1 hour with soft fire.
e. The extract was concentrated by cooling and filtration to leave about 10-50 cc.
f. Adding 5-10 times of alcohol into the concentrated extractive solution.
g. Fractionating the alcohol-containing centella asiatica extract in SFF.
And e, further crystallizing the concentrated solution, wherein the GCMS spectrum of the obtained product is shown in figure 1.
And g, after the SFF fractionation, the GCMS spectra of the products at the bottoms of the first SFF fractionation tank, the second SFF fractionation tank and the SFF extraction tank are shown in figures 2-4.
Example 2
The centella asiatica wine extraction (CE) is prepared by the following steps:
a. firstly, cleaning and drying the centella asiatica.
b. Weighing 1000 g of root of Leptoradix Tripterygii Hypoglauci in an ultrasonic extraction pot.
c. 3000cc of alcohol was added into the ultrasonic extraction pot, and ultrasonic extraction was performed for 1 hour.
d. The extract was concentrated by filtration, leaving about 500-1000 cc.
e. Fractionating the alcohol-containing centella asiatica extract in SFF.
And d, further crystallizing the concentrated solution in the step d, and obtaining a product with a GCMS (general chemical vapor deposition) spectrum shown in figure 5.
And g, after SFF fractionation, the GCMS spectra of the products at the bottoms of the first SFF fractionation tank and the SFF extraction tank are shown in figures 6-7.
Example 3
The liquid propane extraction (CP) of the centella asiatica comprises the following preparation steps:
a. the centella asiatica is cleaned and dried, and then crushed into powder with the particle size of 0.5-5 mm.
b. The 350 g of the root powder of the Hercules crassifolia Hemsl is put into an extraction tank (the tank body is 2L).
c. The operating pressure is 0.40MPa, the temperature is 50 ℃, and alcohol with the volume of 5-10% of that of propane is added.
d. Collecting the extract of centella asiatica containing alcohol in the separation tank to obtain 80-200cc of centella asiatica extract.
e. Subjecting 80-200cc of the extract of centella asiatica containing alcohol to SFF fractionation.
And d, further crystallizing the centella asiatica extract in the step d, wherein the GCMS spectrum of the obtained product is shown in figure 8.
And e, after SFF fractionation, the GCMS spectra of the products at the bottoms of the first SFF fractionation tank, the second SFF fractionation tank and the SFF extraction tank are shown in figures 9-10.
It should be noted that the same extraction results can be obtained by using the device of example 3 with the device for extracting the asiaticoside-rich composition from centella asiatica provided by any of the above examples of the present invention. However, the device for extracting the asiaticoside-rich composition from centella asiatica (fig. 13a) provided by the embodiment of the present invention can be operated at a lower cost.
The SFF fractionation conditions for examples 1 to 3 are shown in Table 1 below.
Table 1:
the content of the asiaticoside composition obtained in examples 1 to 3 is shown in Table 2 below.
Table 2:
the results in table 2 show that the asiaticoside content in the obtained extract is low regardless of water extraction, alcohol extraction and liquid propane extraction, and the asiaticoside content in the product is significantly increased by further supercritical fractionation of the extract.
Furthermore, the combination of subcritical liquid propane and supercritical fractionation is preferred, which results in higher extraction yield, higher asiaticoside content, and lower cost operation in cooperation with the above (SPE + SFF) extraction apparatus (FIG. 13a), and thus is of great industrial value.
Further, the GCMS spectrum 5 of the asiaticoside composition obtained by extracting centella asiatica with wine in example 2 was analyzed, and the results are shown in table 3.
Table 3:
the GCMS spectrum of the asiaticoside composition obtained by extracting centella asiatica with wine in example 2 was analyzed by fig. 6, and the results are shown in table 4.
Table 4:
further, the GCMS 7 of the asiaticoside composition obtained from example 2 by extracting centella asiatica with wine and then subjecting the centella asiatica to supercritical fractionation, and the bottom of SFF extraction tank was analyzed for its components, and the results are shown in table 5.
TABLE 5
The GCMS chart 8 of the product obtained by crystallizing the centella asiatica extract obtained in step d of example 3 was further analyzed for components, and the data are shown in table 6.
Table 6:
the GCMS spectrum 9 of the product from the first SFF fractionator of example 3 was further analyzed for composition and the data are shown in table 7.
Table 7:
the GCMS spectrum 10 of the product from the second SFF fractionator of example 3 was further analyzed for composition and the data are shown in table 8.
Table 8:
examples 4 to 15
Similar to example 3, but under different subcritical extraction conditions (SPE), 0.5MPa, 50 deg.C, the final asiaticoside composition content is as shown in Table 9 below.
Table 9:
| sample (I) | Asiaticoside content (%) |
| Supercritical fractionation first separation tank (CPSFF1st) of centella asiatica liquid propane extract | 18 |
| Supercritical fractionation second separation tank (CPSFF2nd) for liquid propane extract of centella asiatica | 22 |
According to the experiment of the inventor, the pressure of the SPE extraction tank is preferably 0.2-0.5 MPa, more preferably 0.3-0.45 MPa, and even more preferably 0.4 MPa; the temperature of the SPE extraction tank is 30-60 ℃, preferably 40-55 ℃, and more preferably 50 ℃.
In the above embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
While the invention has been described with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method for extracting a composition rich in asiaticoside from centella asiatica root is characterized by comprising the following steps:
s1, cleaning and drying the centella asiatica, and adding an extraction solvent for extraction to obtain centella asiatica extract;
s2, performing supercritical fractionation on the centella asiatica extract, wherein the supercritical fractionation hardware at least comprises an SFF extraction tank, a first SFF fractionation tank and a second SFF fractionation tank;
the supercritical fractionation conditions are as follows: the pressure of the SFF extraction tank is 75-300 bar, and the temperature is 32-100 ℃; the pressure of the first SFF fractionating tank is 70-150 bar, the temperature is 32-100 ℃, the pressure of the second SFF fractionating tank is 40-200 bar, and the temperature is 32-100 ℃.
2. The method of claim 1, wherein the extraction solvent is subcritical propane, and the step of S1 is as follows:
cleaning and drying centella asiatica, and crushing to obtain centella asiatica root powder;
pouring the centella asiatica root powder into an SPE extraction tank of a subcritical propane fluid extraction device for subcritical propane fluid extraction;
introducing the extraction fluid into an SPE separation tank;
removing propane in the SPE separation tank to obtain a centella asiatica extract;
the subcritical propane fluid extraction conditions were: the pressure of the SPE extraction tank is 0.2-0.5 Mpa, and the temperature is 30-60 ℃.
3. The method of claim 2, wherein the propane flow rate is 0.7-1 times the volume of the SPE extraction tank.
4. The method of claim 2, wherein the particle size of the centella asiatica powder is 0.5-5 mm.
5. The method of claim 2, wherein the subcritical propane fluid extraction conditions are: the pressure of the SPE extraction tank is 0.3-0.45 Mpa, and the temperature is 40-55 ℃.
6. The method of claim 2, wherein the subcritical propane fluid extraction step further comprises adding 5-10% by volume of an extraction solvent to the alcohol for co-extraction.
7. The method of claim 1, wherein the extraction solvent is water, and the step of S1 is as follows:
cleaning and drying centella asiatica, adding 2-4 times of water by mass, and extracting at 90-110 ℃ for 0.5-1.5h to obtain an extract;
cooling the extract to room temperature, concentrating and filtering to obtain a concentrated solution;
adding 5-10 times of alcohol into the concentrated solution for dilution to obtain the centella asiatica extract.
8. The method of claim 1, wherein the extraction solvent is alcohol, and the step of S1 is as follows:
cleaning and drying centella asiatica, adding 2-4 times of alcohol by mass, and performing ultrasonic extraction for 0.5-1.5h to obtain an extract;
and filtering the extract, and concentrating to 1/6-1/3 of the volume of the alcohol to obtain the centella asiatica extract.
9. The method of claim 1, wherein the supercritical fractionation conditions are: the pressure of the SFF extraction tank is 85-200 bar, and the temperature is 32-80 ℃; the pressure of the first SFF fractionating tank is 70-120 bar, the temperature is 32-80 ℃, the pressure of the second SFF fractionating tank is 40-100 bar, and the temperature is 32-80 ℃.
10. The method of claim 9, wherein the supercritical fractionation conditions are: the pressure of the SFF extraction tank is 90-210 bar, and the temperature is 40-80 ℃; the pressure of the first SFF fractionating tank is 74-120 bar, and the temperature is 40-80 ℃; the pressure of the second SFF fractionating tank is 44-100 bar, and the temperature is 40-80 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110135003.6A CN112957764A (en) | 2021-01-29 | 2021-01-29 | Method for extracting asiaticoside-rich composition from centella asiatica |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110135003.6A CN112957764A (en) | 2021-01-29 | 2021-01-29 | Method for extracting asiaticoside-rich composition from centella asiatica |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112957764A true CN112957764A (en) | 2021-06-15 |
Family
ID=76272831
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110135003.6A Pending CN112957764A (en) | 2021-01-29 | 2021-01-29 | Method for extracting asiaticoside-rich composition from centella asiatica |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112957764A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090122049A (en) * | 2008-05-23 | 2009-11-26 | 한국과학기술연구원 | Extraction and separation of asiatic acid and asiaticoside from centella asiatica using subcritical water |
| CN102532244A (en) * | 2011-12-31 | 2012-07-04 | 广西大学 | Method for preparing high-purity asiaticosid |
| CN103796631A (en) * | 2012-06-29 | 2014-05-14 | 生物光谱公司 | Compositions for whitening skin comprising madecassoside |
| CN107098947A (en) * | 2017-04-28 | 2017-08-29 | 南宁馨艺荣生物科技有限公司 | A kind of technique that Asiaticoside is extracted from centella |
| CN111228851A (en) * | 2020-01-14 | 2020-06-05 | 三益创价生物科技(深圳)有限公司 | Method and device for extracting composition rich in cinnamaldehyde from cinnamon bark |
-
2021
- 2021-01-29 CN CN202110135003.6A patent/CN112957764A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090122049A (en) * | 2008-05-23 | 2009-11-26 | 한국과학기술연구원 | Extraction and separation of asiatic acid and asiaticoside from centella asiatica using subcritical water |
| CN102532244A (en) * | 2011-12-31 | 2012-07-04 | 广西大学 | Method for preparing high-purity asiaticosid |
| CN103796631A (en) * | 2012-06-29 | 2014-05-14 | 生物光谱公司 | Compositions for whitening skin comprising madecassoside |
| CN107098947A (en) * | 2017-04-28 | 2017-08-29 | 南宁馨艺荣生物科技有限公司 | A kind of technique that Asiaticoside is extracted from centella |
| CN111228851A (en) * | 2020-01-14 | 2020-06-05 | 三益创价生物科技(深圳)有限公司 | Method and device for extracting composition rich in cinnamaldehyde from cinnamon bark |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103923152B (en) | A kind of extracting method of mogroside V | |
| CN103920305B (en) | A kind of method of pot group type counter-flow extraction Chinese caterpillar fungus | |
| CN104120037A (en) | Extracting method for jasmine flower essential oil | |
| CN1263394C (en) | Method of combined preparing garlic essential oil and garlic polysaccharide | |
| CN108383890B (en) | Preparation method of high-content ginsenoside Re extract | |
| CN106800586A (en) | A kind of method of Moringa protein high efficiency extraction | |
| CN105311075A (en) | Preparation method of manyprickle acanthopanax root extract | |
| CN110892987A (en) | Preparation method of wolfberry syrup | |
| CN110496179A (en) | A kind of method and application for rapidly and efficiently extracting antioxidant in Areca | |
| CN106832037A (en) | A kind of notoginseng polysaccharide extracting method rapidly and efficiently | |
| CN105693678A (en) | Method for extracting procyanidine from grape seeds | |
| CN112957764A (en) | Method for extracting asiaticoside-rich composition from centella asiatica | |
| CN105748524A (en) | Method for separating and purifying functional components in placenta by supercritical fluid technology | |
| CN102180991B (en) | Comprehensive utilization method of pumpkin | |
| CN108338999A (en) | A kind of preparation method of sanchi leaf total saposins | |
| CN107287026B (en) | Deacidifying extraction method for peony seed oil | |
| CN1266160C (en) | Process for extracting rubusoside of fruit of Gorsvenor Momordica | |
| CN101987856A (en) | Preparation method of anthocyanin monomer cornflower-3-glucoside | |
| CN105038946A (en) | Peony essential oil supercritical CO2 extraction method | |
| CN110746470B (en) | Method for extracting phenylethanoid glycosides from cistanche tubulosa by ionic liquid aqueous two-phase extraction | |
| CN1067688C (en) | Process and apparatus for producing pectine by pre-acidolysis and continuous high-acidity extraction | |
| CN114107418A (en) | Preparation method of ginseng polypeptide | |
| CN105420293A (en) | Method for separating and purifying resveratrol from traditional Chinese medicine polygonum cuspidatum extraction solution | |
| CN1312168C (en) | Puerarin preparing process | |
| CN105395583A (en) | Preparing method for acanthopanax senticosus extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210615 |
|
| RJ01 | Rejection of invention patent application after publication |