CN105125599B - A kind of preparation method of the tribulus terrestris extraction containing total saponins of tribulus - Google Patents
A kind of preparation method of the tribulus terrestris extraction containing total saponins of tribulus Download PDFInfo
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- MUKYLHIZBOASDM-UHFFFAOYSA-N 2-[carbamimidoyl(methyl)amino]acetic acid 2,3,4,5,6-pentahydroxyhexanoic acid Chemical compound NC(=N)N(C)CC(O)=O.OCC(O)C(O)C(O)C(O)C(O)=O MUKYLHIZBOASDM-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229930182490 saponin Natural products 0.000 title claims abstract description 24
- 150000007949 saponins Chemical class 0.000 title claims abstract description 24
- 235000017709 saponins Nutrition 0.000 title claims abstract description 24
- 241000819233 Tribulus <sea snail> Species 0.000 title claims abstract description 23
- 238000000605 extraction Methods 0.000 title claims abstract description 23
- 229940047183 tribulus Drugs 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 241001521901 Tribulus lanuginosus Species 0.000 title claims abstract 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000004952 Polyamide Substances 0.000 claims abstract description 16
- 229920002647 polyamide Polymers 0.000 claims abstract description 16
- 235000021419 vinegar Nutrition 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000009835 boiling Methods 0.000 claims abstract description 13
- 239000000052 vinegar Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 49
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 25
- 239000003480 eluent Substances 0.000 claims description 25
- 239000000741 silica gel Substances 0.000 claims description 25
- 229910002027 silica gel Inorganic materials 0.000 claims description 25
- 229960001866 silicon dioxide Drugs 0.000 claims description 25
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 21
- 235000019441 ethanol Nutrition 0.000 claims description 20
- 239000000047 product Substances 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 11
- 229920005989 resin Polymers 0.000 claims description 11
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 claims description 10
- 238000010828 elution Methods 0.000 claims description 10
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 7
- 239000012043 crude product Substances 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 6
- 238000004587 chromatography analysis Methods 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000001764 infiltration Methods 0.000 claims description 5
- 230000008595 infiltration Effects 0.000 claims description 5
- 239000012044 organic layer Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 230000006837 decompression Effects 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- 238000004440 column chromatography Methods 0.000 abstract description 2
- 238000003810 ethyl acetate extraction Methods 0.000 abstract description 2
- 238000010898 silica gel chromatography Methods 0.000 abstract 1
- 241001533104 Tribulus terrestris Species 0.000 description 28
- 239000000243 solution Substances 0.000 description 23
- 238000010025 steaming Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 102000004190 Enzymes Human genes 0.000 description 7
- 108090000790 Enzymes Proteins 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- MUMGGOZAMZWBJJ-DYKIIFRCSA-N Testostosterone Chemical compound O=C1CC[C@]2(C)[C@H]3CC[C@](C)([C@H](CC4)O)[C@@H]4[C@@H]3CCC2=C1 MUMGGOZAMZWBJJ-DYKIIFRCSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000001925 catabolic effect Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 150000005856 steroid saponins Chemical class 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 102000009151 Luteinizing Hormone Human genes 0.000 description 2
- 108010073521 Luteinizing Hormone Proteins 0.000 description 2
- 230000003712 anti-aging effect Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 150000002338 glycosides Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000003808 methanol extraction Methods 0.000 description 2
- 210000003205 muscle Anatomy 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000028327 secretion Effects 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 229960003604 testosterone Drugs 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- DVGGLGXQSFURLP-VWMSDXGPSA-N tribuloside Chemical compound C([C@@H]1[C@H]([C@@H]([C@@H](O)[C@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=CC(O)=CC=2)=O)O1)O)O)OC(=O)\C=C\C1=CC=C(O)C=C1 DVGGLGXQSFURLP-VWMSDXGPSA-N 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000009777 vacuum freeze-drying Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 240000006122 Chenopodium album Species 0.000 description 1
- 235000009344 Chenopodium album Nutrition 0.000 description 1
- 241001529246 Platymiscium Species 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Abstract
The present invention provides a kind of preparation methods of tribulus terrestris extraction, include the following steps：Raw material heap buried, ethyl acetate extraction, polyamide column chromatography and dry silica gel column chromatography, micro-wave vacuum after vinegar water boiling, finally obtain the tribulus terrestris extraction that total saponins of tribulus content is more than 95 wt.%.
Description
Technical field
The present invention relates to a kind of preparation methods of tribulus terrestris extraction, belong to natural plant extracts field.
Background technology
Tribulus terrestris（Tribulus terrestris L.) it is zygophyllaceae puncture vine platymiscium, it is annual climing plant, again
Claim tribulus terrestris, tribulus terrestris.In recent years, with deepening continuously to the research of tribulus terrestris, isolated flavones, life from the plant
The chemical compositions such as alkaloids, organic acid, polysaccharide and steroid saponin, wherein more with the research of steroid saponin constituents.
Steroid saponin is the principle active component of tribulus terrestris, research shows that tribuloside constituents can stimulate human body to hang down
The secretion of body interstitialcellstimulating hormone (ICSH) promotes the secretion of testosterone, improves internal plasma testosterone level, increases muscle strength, promotes muscle power
Restore, the sportsman for widely increasing myokinesis person and other sports class sports items for bodybuilding uses in training.In addition, in recent years
It also found that tribuloside has the effects that hypoglycemic, anti-aging, adjusting blood fat, antibacterial, anticancer to study, and contained by it
Peroxide decomposition enzyme also have the function of apparent anti-aging, it is anti-oxidant, lessen fatigue, be highly suitable as daily life health care
Product.
Currently, it is pure through macroreticular resin again to extract total saponins of tribulus generally use high concentration ethanol extraction with aqueous solution from tribulus terrestris
Change to refine and form, also it is proposed that using the refined method of methanol extraction alumina column after enzymolysis, or even there is researcher to carry
Go out first to extract the total saponins of tribulus catabolic enzyme that tribulus terrestris itself contains, then itself enzyme with the catabolic enzyme enzymolysis and extraction total saponins of tribulus
Solution.But all there are various disadvantages in above-mentioned various methods, as ethanol water extraction is difficult to obtain the puncture vine soap of high-purity
Glycosides, after enzymolysis methanol extraction used toxic solvent, there is the complicated step for obtaining catabolic enzyme in advance in itself enzymatic isolation method, and decompose
Enzyme is difficult to expeditiously to obtain, etc..Therefore, present inventor, in conjunction with many experiments, is proposed a kind of by concentrating on studies
With the preparation method of total saponins of tribulus tribulus terrestris extraction as main component, this method is at low cost, high income, does not use toxic examination
Agent is easy to industrialization.
Invention content
To achieve the goals above, the present invention provides a kind of with total saponins of tribulus tribulus terrestris extraction as main component
Preparation method includes the following steps：
（1）Take tribulus terrestris raw material, water proof boiling 0.5-2 hours that vinegar is added in water, it is natural heap buried 1-4 hours after boiling
It is cooling；
（2）5-8 times of ethyl acetate is added into the raw material after infiltration, extracts 1-2 hours, filtering obtains extracting solution；
（3）Extracting solution is taken, adjusts pH to neutrality, is concentrated under reduced pressure, by polyamide chromatography post separation, applied sample amount and polyamide ratio
It is 1: 5-1: 25, resin column blade diameter length ratio is 1: 4-1: 15, respectively with 1-10 times of cylinder ponding, 5-10 times of column volume 20%-40%
Ethanol solution elution removal of impurities, then eluted with 4-12 times of column volume 40%-90% ethanol solution, collect washing for 40%-90% ethyl alcohol
De- liquid, is recovered under reduced pressure ethyl alcohol and concentrates；
（4）PH to 4.0-6.0 is adjusted, with 1-8 times of t-butyl methyl ether measured of solution, divides 2-6 extraction, detaches organic layer,
T-butyl methyl ether is recovered under reduced pressure, is added 1-3 times and measures silica gel, stirs, volatilizes；
（5）Stirring sample silica gel is added on the dry silicagel column that 5-20 times installed is measured, silicagel column blade diameter length ratio is 1: 4-1:
15, using 50% ethyl alcohol-t-butyl methyl ether as eluant, eluent, gradient elution, collect 50% ethyl alcohol-t-butyl methyl ether (4: 6) to (6:
4) eluent of section；
（6）The eluant, eluent in eluent is recovered under reduced pressure, obtains crude product；
（7）5-20 times of 50% ethanol water dissolving is added, micro-wave vacuum obtains product.
Wherein, step（1）In, the addition of vinegar is preferably the 3-10wt% of the weight of water, more preferable 6-8%；
Wherein, step（7）In, micro-wave vacuum temperature：40-60 DEG C, 2-4 DEG C of return difference temperature, vacuum degree -0.07Mpa
More than, microwave power 10-80KW is 30-80 minutes dry.
The present invention also provides the tribulus terrestris extractions made from above-mentioned preparation method, including concentration is more than 95 wt.%'s
Total saponins of tribulus.
Compared with prior art, the present invention pre-treatment step is increased before the extraction processing of medicinal material, with the water containing vinegar
Boiling raw material simultaneously gives the enough heap buried time；According to the dissolution characteristics of total saponins of tribulus, select ethyl acetate as Extraction solvent,
Extract step；And screening and optimization Jing Guo system, it is determined that polyamide resin column combines the polishing purification of dry silicagel column
Step, separating effect is splendid, and through microwave drying, and in finally obtained tribulus terrestris extraction, total saponins of tribulus concentration is more than 95
Wt.%, better than existing various preparation methods in the prior art.Entire method material therefor is conventional material, at low cost and receipts
Rate is high and solvent is Ke Xunhuanliyong, can reduce environmental pollution, be easy to industrialization.
Present inventor has carried out a large number of experiments, because factor needed to be considered is too many and screening process repeatedly, under
Text only provides part of test results.Wherein, the method that the method for measuring total saponins of tribulus is known in the art, may be used UV methods,
HPLC methods etc., design parameter no longer arrange in detail.
1, medicinal material pre-treating technology
Experiment material：Tribulus terrestris, ethyl acetate, vinegar, water, salt
Experimental method：Tribulus terrestris is taken, 7 groups of equivalent, respectively control group are divided into（Without any pre-treatment）, water steaming group 1
（Steam by water bath 1h）, vinegar water steaming group 1（Steam by water bath 1h）, saline solution steaming group 1（Steam by water bath 1h）, water steaming group 2（Heap buried after Steam by water bath 1h
2 hours）, vinegar water steaming group 2（Heap buried 2 hours after Steam by water bath 1h）, saline solution steaming group 2（Heap buried 2 hours after Steam by water bath 1h）, natural
After cooling, respectively with 6 times of amount ethyl acetate extractions, the content of total saponins of tribulus in solution is measured.
Experimental result is shown in Table one
The screening of one pre-treating technology of table
| Total saponins of tribulus（mg/100ml） | |
| Control group | 13.22 |
| Water steaming group 1 | 15.17 |
| Vinegar water steaming group 1 | 22.07 |
| Saline solution steaming group 1 | 14.35 |
| Water steaming group 2 | 18.54 |
| Vinegar water steaming group 2 | 30.89 |
| Saline solution steaming group 2 | 20.21 |
It can be seen that after vinegar water boiling and carrying out the raw material of heap buried processing in solvent extraction stage for total saponins of tribulus
It dissolves out highly beneficial.Its reason is unknown, but inventor's conjecture is that certain effect has occurred in the enzyme that tribulus terrestris raw material contains so that puncture
Lamb's-quarters saponin(e is easier to dissolve out.
2, the screening polyamide column chromatography purifying of purification step
Macroreticular resin D101 is widely used in the prior art and carries out isolating and purifying for total saponins of tribulus, the present inventor to this also into
Careful research is gone.
Experimental method：Take step of the present invention（2）Obtained extracting solution after concentration, has investigated various kinds of resin respectively, including
D101, D311, AB-8, polyamide, LH-20, dry silicagel column etc., and according to the situation detached for the first time, carried out the group of resin column
It closes and uses, including macroreticular resin is combined polyamide, macroreticular resin is combined dry silicagel column, and polyamide is combined dry silicagel column etc., into one
It walks and applicable eluant, eluent is carried out preferably.Final result shows that polyamide column is combined dry silicagel column, and using recorded in the present invention
Eluant, eluent, the separative efficiency of optimal total saponins of tribulus can be obtained.
3, drying means is studied
Experimental method：Take the method for the present invention step（6）The crude product obtained, after 8 times of 50% ethanol water dissolving is added, point
Cai Yong not be dried in vacuo, vacuum freezedrying, spray drying, micro-wave vacuum, obtain product, measure the puncture vine soap in product
Glycosides content, as a result see the table below.
Three drying means result of study of table
| Vacuum drying | Vacuum freezedrying | Spray drying | Micro-wave vacuum | |
| Total saponins of tribulus content | 95.17 | 96.58 | 95.14 | 98.01 |
| Moisture | 1.82 | 1.37 | 2.21 | 0.79 |
| Drying time | 1h | 1h | 1h | 1h |
| Dissolvent residual | Nothing | Nothing | 1.5 | Nothing |
The result shows that：Tribulus terrestris extraction rich in total saponins of tribulus preferably uses microwave vacuum drying process, and effect is best,
Treating capacity is big, and drying temperature is low, and the time is short, and products obtained therefrom index is good.
Embodiment 1
A kind of preparation method of tribulus terrestris extraction, includes the following steps：
（1）Take tribulus terrestris raw material, water proof boiling 1 hour that 8wt.% vinegars are added in water, heap buried 2 hours after boiling are natural
It is cooling；
（2）6 times of ethyl acetate are added into the raw material after infiltration, extract 2 hours, filtering obtains extracting solution；
（3）Extracting solution is taken, adjusts pH to neutrality, is concentrated under reduced pressure, by polyamide chromatography post separation, applied sample amount and polyamide ratio
It is 1: 20, resin column blade diameter length ratio is 1: 10, is cleaned respectively with 5 times of cylinder ponding, 5 times of 20% ethanol solution of column volume elutions, then
It is eluted with 10 times of 50% ethanol solutions of column volume, collects the eluent of 50% ethyl alcohol, ethyl alcohol is recovered under reduced pressure and concentrates；
（4）PH to 5.0 or so is adjusted, with the t-butyl methyl ether of 5 times of amounts of solution, point 3 extractions detach organic layer, decompression
T-butyl methyl ether is recycled, 3 times of amount silica gel are added, stirring volatilizes；
（5）Stirring sample silica gel being added on the dry silicagel column of the 15 times of amounts installed, silicagel column blade diameter length ratio is 1: 10, with
50% ethyl alcohol-t-butyl methyl ether is eluant, eluent, and gradient elution collects 50% ethyl alcohol-t-butyl methyl ether (4: 6) to (6: 4) section
Eluent；
（6）The eluant, eluent in eluent is recovered under reduced pressure, obtains crude product；
（7）10 times of 50% ethanol water dissolving, micro-wave vacuum is added（Micro-wave vacuum temperature：40 DEG C, return difference
4 DEG C, vacuum degree -0.07Mpa or more, microwave power 80KW of temperature, dry 1h）, product is obtained, after testing, total saponins of tribulus in product
Content is 97.21 wt.%.
Embodiment 2
A kind of preparation method of tribulus terrestris extraction, includes the following steps：
（1）Take tribulus terrestris raw material, water proof boiling 1 hour that 5wt.% vinegars are added in water, heap buried 2 hours after boiling are natural
It is cooling；
（2）5 times of ethyl acetate are added into the raw material after infiltration, extract 2 hours, filtering obtains extracting solution；
（3）Extracting solution is taken, adjusts pH to neutrality, is concentrated under reduced pressure, by polyamide chromatography post separation, applied sample amount and polyamide ratio
It is 1: 20, resin column blade diameter length ratio is 1: 10, is cleaned respectively with 5 times of cylinder ponding, 5 times of 30% ethanol solution of column volume elutions, then
It is eluted with 10 times of 75% ethanol solutions of column volume, collects the eluent of 75% ethyl alcohol, ethyl alcohol is recovered under reduced pressure and concentrates；
（4）PH to 5.0 or so is adjusted, with the t-butyl methyl ether of 7 times of amounts of solution, point 3 extractions detach organic layer, decompression
T-butyl methyl ether is recycled, 2 times of amount silica gel are added, stirring volatilizes；
（5）Stirring sample silica gel being added on the dry silicagel column of the 10 times of amounts installed, silicagel column blade diameter length ratio is 1: 15, with
50% ethyl alcohol-t-butyl methyl ether is eluant, eluent, and gradient elution collects 50% ethyl alcohol-t-butyl methyl ether (4: 6) to (6: 4) section
Eluent；
（6）The eluant, eluent in eluent is recovered under reduced pressure, obtains crude product；
（7）12 times of 50% ethanol water dissolving, micro-wave vacuum is added（Micro-wave vacuum temperature：50 DEG C, return difference
3 DEG C, vacuum degree -0.07Mpa or more, microwave power 60KW of temperature, dry 1h）, product is obtained, after testing, total saponins of tribulus in product
Content is 98.52 wt.%.
Embodiment 3
A kind of preparation method of tribulus terrestris extraction, includes the following steps：
（1）Take tribulus terrestris raw material, water proof boiling 1 hour that 10wt.% vinegars are added in water, heap buried 1 hour after boiling is natural
It is cooling；
（2）8 times of ethyl acetate are added into the raw material after infiltration, extract 2 hours, filtering obtains extracting solution；
（3）Extracting solution is taken, adjusts pH to neutrality, is concentrated under reduced pressure, by polyamide chromatography post separation, applied sample amount and polyamide ratio
It is 1: 15, resin column blade diameter length ratio is 1: 10, is cleaned respectively with 5 times of cylinder ponding, 10 times of 30% ethanol solution of column volume elutions, then
It is eluted with 10 times of 70% ethanol solutions of column volume, collects the eluent of 70% ethyl alcohol, ethyl alcohol is recovered under reduced pressure and concentrates；
（4）PH to 4.0 or so is adjusted, with the t-butyl methyl ether of 8 times of amounts of solution, point 3 extractions detach organic layer, decompression
T-butyl methyl ether is recycled, 3 times of amount silica gel are added, stirring volatilizes；
（5）Stirring sample silica gel is added on the dry silicagel column of the 10 times of amounts installed, silicagel column blade diameter length ratio is 1: 8, with 50%
Ethyl alcohol-t-butyl methyl ether is eluant, eluent, and gradient elution collects 50% ethyl alcohol-t-butyl methyl ether (4: 6) washing to (6: 4) section
De- liquid；
（6）The eluant, eluent in eluent is recovered under reduced pressure, obtains crude product；
（7）8 times of 50% ethanol water dissolving, micro-wave vacuum is added（Micro-wave vacuum temperature：60 DEG C, return difference temperature
3 DEG C, vacuum degree -0.07Mpa or more, microwave power 70KW of degree, dry 1h）, product is obtained, after testing, total saponins of tribulus contains in product
Amount is 98.66 wt.%.
Claims (5)
1. the preparation method of tribulus terrestris extraction, which is characterized in that include the following steps：
（1）Take tribulus terrestris raw material, water proof boiling 0.5-2 hours that vinegar is added in water, it is naturally cold heap buried 1-4 hours after boiling
But；
（2）5-8 times of ethyl acetate is added into the raw material after infiltration, extracts 1-2 hours, filtering obtains extracting solution；
（3）Extracting solution is taken, adjusts pH to neutrality, is concentrated under reduced pressure, by polyamide chromatography post separation, applied sample amount is 1 with polyamide ratio:
5-1: 25, resin column blade diameter length ratio is 1: 4-1: 15, respectively with 1-10 times of cylinder ponding, 5-10 times of column volume 20%-40% ethyl alcohol
Solution elution removal of impurities, then eluted with 4-12 times of column volume 40%-90% ethanol solution, the eluent of 40%-90% ethyl alcohol is collected,
Ethyl alcohol is recovered under reduced pressure and concentrates；
（4）PH to 4.0-6.0 is adjusted, with 1-8 times of t-butyl methyl ether measured of solution, divides 2-6 extraction, detaches organic layer, decompression
T-butyl methyl ether is recycled, 1-3 times is added and measures silica gel, stirs, volatilizes；
（5）Stirring sample silica gel being added on the dry silicagel column that 5-20 times installed is measured, silicagel column blade diameter length ratio is 1: 4-1: 15, with
50% ethyl alcohol-t-butyl methyl ether is eluant, eluent, and gradient elution collects the 50% ethyl alcohol-tertbutyl methyl that ratio is 4: 6 to 6: 4
The eluent of ether section；
（6）The eluant, eluent in eluent is recovered under reduced pressure, obtains crude product；
（7）5-20 times of 50% ethanol water dissolving is added, micro-wave vacuum obtains product, and total saponins of tribulus content is big in the product
In 95 wt%.
2. preparation method as described in claim 1, which is characterized in that step（1）In, the addition of vinegar is the weight of water
3-10wt%。
3. preparation method as claimed in claim 2, which is characterized in that step（1）In, the addition of vinegar is the weight of water
6-8wt%。
4. preparation method as claimed in claim 1 or 2, which is characterized in that step（7）In, micro-wave vacuum temperature：40-
60 DEG C, 2-4 DEG C, vacuum degree -0.07Mpa or more, microwave power 10-80KW of return difference temperature is 30-80 minutes dry.
5. tribulus terrestris extraction made from the preparation method as described in claim 1-4 any one.
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| CN106317160A (en) * | 2016-07-26 | 2017-01-11 | 西安岳达生物科技股份有限公司 | Tribulus terrestris saponin K extracting and separating method |
| CN110227047B (en) * | 2019-06-26 | 2022-05-13 | 广州三广生物科技有限公司 | Skin care composition with effect of removing red blood streak and preparation method thereof |
| CN111494440A (en) * | 2020-04-24 | 2020-08-07 | 武汉轻工大学 | Extraction, purification and preparation technology of blood sugar reducing component saponin in caltrop, caltrop saponin extract and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102178706A (en) * | 2011-01-24 | 2011-09-14 | 南京泽朗医药科技有限公司 | Method for extracting tribuloside |
| CN103040880A (en) * | 2012-12-13 | 2013-04-17 | 大兴安岭林格贝有机食品有限责任公司 | Separation and purification method of tribulus terrestris saponin |
| DE112012003484T5 (en) * | 2011-08-23 | 2014-05-15 | Mustafa Eraslan | Tribulus terrestris, Avena sativa and Panax ginseng extract combination |
-
2015
- 2015-08-14 CN CN201510498286.5A patent/CN105125599B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102178706A (en) * | 2011-01-24 | 2011-09-14 | 南京泽朗医药科技有限公司 | Method for extracting tribuloside |
| DE112012003484T5 (en) * | 2011-08-23 | 2014-05-15 | Mustafa Eraslan | Tribulus terrestris, Avena sativa and Panax ginseng extract combination |
| CN103040880A (en) * | 2012-12-13 | 2013-04-17 | 大兴安岭林格贝有机食品有限责任公司 | Separation and purification method of tribulus terrestris saponin |
Non-Patent Citations (1)
| Title |
|---|
| 正交试验法优选刺蒺藜皂苷的提取工艺;王霄？等;《西北药学杂志》;20080115;第23卷(第01期);24-26 * |
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