WO2017181303A1 - 东革阿里有效成分的制备方法及其用途 - Google Patents
东革阿里有效成分的制备方法及其用途 Download PDFInfo
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- WO2017181303A1 WO2017181303A1 PCT/CN2016/000216 CN2016000216W WO2017181303A1 WO 2017181303 A1 WO2017181303 A1 WO 2017181303A1 CN 2016000216 W CN2016000216 W CN 2016000216W WO 2017181303 A1 WO2017181303 A1 WO 2017181303A1
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- tongkat ali
- active ingredient
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- 239000004480 active ingredient Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 17
- 240000005739 Eurycoma longifolia Species 0.000 title claims abstract description 6
- 239000011347 resin Substances 0.000 claims abstract description 19
- 229920005989 resin Polymers 0.000 claims abstract description 19
- 239000012528 membrane Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 201000005569 Gout Diseases 0.000 claims abstract description 9
- 230000002929 anti-fatigue Effects 0.000 claims abstract description 9
- 230000036299 sexual function Effects 0.000 claims abstract description 9
- 230000035558 fertility Effects 0.000 claims abstract description 8
- 230000036039 immunity Effects 0.000 claims abstract description 8
- 230000002708 enhancing effect Effects 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000000284 extract Substances 0.000 claims description 12
- 238000001179 sorption measurement Methods 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 102000002068 Glycopeptides Human genes 0.000 claims description 6
- 108010015899 Glycopeptides Proteins 0.000 claims description 6
- 150000001413 amino acids Chemical class 0.000 claims description 6
- 230000006870 function Effects 0.000 claims description 6
- 150000004676 glycans Chemical class 0.000 claims description 6
- 229920005610 lignin Polymers 0.000 claims description 6
- 229920001282 polysaccharide Polymers 0.000 claims description 6
- 239000005017 polysaccharide Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000002137 ultrasound extraction Methods 0.000 claims description 6
- 238000003809 water extraction Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000011282 treatment Methods 0.000 claims description 4
- DQJCDTNMLBYVAY-ZXXIYAEKSA-N (2S,5R,10R,13R)-16-{[(2R,3S,4R,5R)-3-{[(2S,3R,4R,5S,6R)-3-acetamido-4,5-dihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy}-5-(ethylamino)-6-hydroxy-2-(hydroxymethyl)oxan-4-yl]oxy}-5-(4-aminobutyl)-10-carbamoyl-2,13-dimethyl-4,7,12,15-tetraoxo-3,6,11,14-tetraazaheptadecan-1-oic acid Chemical compound NCCCC[C@H](C(=O)N[C@@H](C)C(O)=O)NC(=O)CC[C@H](C(N)=O)NC(=O)[C@@H](C)NC(=O)C(C)O[C@@H]1[C@@H](NCC)C(O)O[C@H](CO)[C@H]1O[C@H]1[C@H](NC(C)=O)[C@@H](O)[C@H](O)[C@@H](CO)O1 DQJCDTNMLBYVAY-ZXXIYAEKSA-N 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000000108 ultra-filtration Methods 0.000 claims description 3
- 239000003480 eluent Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000001471 micro-filtration Methods 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 238000005194 fractionation Methods 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 238000001223 reverse osmosis Methods 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000006286 aqueous extract Substances 0.000 abstract 1
- 230000036314 physical performance Effects 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- 241000196324 Embryophyta Species 0.000 description 7
- 241000699670 Mus sp. Species 0.000 description 6
- 238000011160 research Methods 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 231100000636 lethal dose Toxicity 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 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 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001728 nano-filtration Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 244000166124 Eucalyptus globulus Species 0.000 description 1
- SNGWXAVWKXBHJD-UHFFFAOYSA-N Eurycolactone Natural products CC1C(O)C(O)C2C3(C)C(O)C(O)C=C(C)C3C(OC(=O)C)C4OC(=O)C1C24C SNGWXAVWKXBHJD-UHFFFAOYSA-N 0.000 description 1
- OGHYZHNTIINXEO-MGBQOKOWSA-N Eurycomalactone Chemical compound O[C@@H]([C@]1(C)[C@H]2[C@H]3O)C(=O)C=C(C)[C@@H]1CC(=O)[C@@]2(C)[C@H]1C(=O)O[C@@H]3[C@@H]1C OGHYZHNTIINXEO-MGBQOKOWSA-N 0.000 description 1
- OGHYZHNTIINXEO-ONPJAVPJSA-N Eurycomalactone Natural products O=C1O[C@H]2[C@H](O)[C@@H]3[C@@]4(C)[C@H](O)C(=O)C=C(C)[C@@H]4CC(=O)[C@]3(C)[C@H]1[C@H]2C OGHYZHNTIINXEO-ONPJAVPJSA-N 0.000 description 1
- TYXFVKGQQWDJKA-SREAOFIKSA-N Eurycomaoside Natural products O([C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1)[C@H]1[C@]2(C)[C@@H]3[C@@H](O)[C@H](O)[C@H](C)[C@@H]4C(=O)O[C@H]([C@H](O)[C@H]2[C@](O)(C)C=C1)[C@]34C TYXFVKGQQWDJKA-SREAOFIKSA-N 0.000 description 1
- 206010027304 Menopausal symptoms Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- XOJVVFBFDXDTEG-UHFFFAOYSA-N Norphytane Natural products CC(C)CCCC(C)CCCC(C)CCCC(C)C XOJVVFBFDXDTEG-UHFFFAOYSA-N 0.000 description 1
- 208000001132 Osteoporosis Diseases 0.000 description 1
- UCUWZJWAQQRCOR-UHFFFAOYSA-N Pasakbumin A Natural products O1C(=O)C(O)C2(O)C(=C)C(O)C3(O)C4C5(C)C(O)C(=O)C=C(C)C5CC1C42CO3 UCUWZJWAQQRCOR-UHFFFAOYSA-N 0.000 description 1
- 241000700159 Rattus Species 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 231100000215 acute (single dose) toxicity testing Toxicity 0.000 description 1
- 238000011047 acute toxicity test Methods 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000000078 anti-malarial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- MOCOVNGOINOTNW-FDPUJYPZSA-N chembl1171669 Chemical compound C([C@@]12[C@]3(O)[C@@H](O)C(=O)O[C@H]4[C@]53CO[C@@]([C@@H]2O)(O)[C@@H]5[C@@]2(C)[C@H](O)C(=O)C=C([C@@H]2C4)C)O1 MOCOVNGOINOTNW-FDPUJYPZSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 150000004141 diterpene derivatives Chemical class 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012869 ethanol precipitation Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- UCUWZJWAQQRCOR-OKNZMGBLSA-N eurycomanone Chemical compound O1C(=O)[C@H](O)[C@@]2(O)C(=C)[C@@H](O)[C@@]3(O)[C@@H]4[C@@]5(C)[C@H](O)C(=O)C=C(C)[C@@H]5C[C@@H]1[C@]42CO3 UCUWZJWAQQRCOR-OKNZMGBLSA-N 0.000 description 1
- 239000009947 eurycomanone Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007912 intraperitoneal administration Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron indole ketone Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007721 medicinal effect Effects 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 230000003340 mental effect Effects 0.000 description 1
- 230000008558 metabolic pathway by substance Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- MOCOVNGOINOTNW-UHFFFAOYSA-N pasakbumin-B Natural products C1C2C(C)=CC(=O)C(O)C2(C)C2C(C3O)(O)OCC22C1OC(=O)C(O)C2(O)C13CO1 MOCOVNGOINOTNW-UHFFFAOYSA-N 0.000 description 1
- 231100000915 pathological change Toxicity 0.000 description 1
- 230000036285 pathological change Effects 0.000 description 1
- 230000003285 pharmacodynamic effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 150000003421 squalenes Chemical class 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 235000019640 taste Nutrition 0.000 description 1
- 229960003604 testosterone Drugs 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- 210000001835 viscera Anatomy 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/77—Sapindaceae (Soapberry family), e.g. lychee or soapberry
Definitions
- the invention belongs to the field of plant natural product extraction, and particularly relates to a method for preparing an active ingredient of Tongkat Ali plant and a combined application.
- Eurycoma longifolia is a genus of the genus Eucalyptus, a wild shrub that grows in the moist sandy soil of the pristine rainforest near the equator and is widely distributed in Southeast Asia such as Malaysia, Indonesia, and Vietnam. Modern research shows that Tongkat Ali has a high medicinal value.
- the components obtained by the Tongkat Ali plant according to various treatment methods have anticancer activity, antimalarial activity and sexual function, respectively. In addition, it also has certain effects in reducing blood sugar, antibacterial, treating gout, osteoporosis and the like.
- the chemical constituents isolated from different parts of Tongkat Ali are mainly diterpenoids containing iron lignin skeleton and iron indole ketone alkaloids such as eurycomaoside, eurycolactone, eurycomalactone, eurycomanone and pasakbumin-B. .
- iron lignin skeleton containing iron lignin skeleton and iron indole ketone alkaloids
- eurycomaoside eurycolactone
- eurycomalactone eurycomalactone
- pasakbumin-B pasakbumin-B.
- biphenyl lignin squalene derivatives
- active polysaccharides active polysaccharides
- glycopeptides glycopeptides
- Tongkat Ali plants directly as decoction pieces is more common, but Tongkat Ali brewing has problems such as bitter taste, low pharmacodynamics and low drug utilization. Therefore, it is very important to study the high content of active ingredients in Tongkat Ali, the preparation process is reliable, the medicinal effect is clear, and the taste is good.
- Tongkat Ali extraction mainly adopts solvent reflux extraction or high-temperature water extraction process, such as patent CN104757424A, which is extracted by boiling method; patent US20070224300A1 uses boiling water extraction; “Tongkat Ali's testosterone content, substance metabolism and resistance to exercise training rats The effect of exercise fatigue ability" was prepared by boiling water; the article “Separation and identification of chemical components of Tongkat Ali” was extracted by water reflux.
- Patent CN103408564A extracts Tongkat Ali with organic solvent; the "Experimental Study on Anti-fatigue Effect of Tongkat Ali Extract” uses an alcohol extraction process.
- boiling water extraction and organic solvent extraction methods can decompose or denature various active components in plants, thereby reducing the effect of drugs, and at the same time, energy consumption is high, environmental protection is difficult, and solvent costs are high. Large, the extraction process is highly harmful.
- the invention provides a preparation method of an active ingredient combination of Tongkat Ali with enhanced functions, improved fertility rate, refreshing anti-fatigue, enhancing immunity, increasing physical fitness and relieving gout.
- the method not only uses the ultrasonic aqueous solution to extract the active ingredient but also uses macroporous resin for adsorption separation and membrane separation, retains the biological activity of the active ingredient in the Tongkat Ali plant and selectively enriches it.
- the preparation method of the Tongkat Ali active ingredient mentioned in the present invention is as follows:
- the water extract is filtered and centrifuged to remove the precipitate and directly adsorbed through the macroporous resin. After adsorption, the resin column is eluted by the eluent and the target component is collected, and the impurities are removed by ethanol precipitation, and concentrated and dried to obtain the active ingredient group A of Tongkat Ali;
- the Tongkat Ali active ingredient groups A and B are mixed to prepare a Tongkat Ali active ingredient combination.
- the mass-to-volume ratio of Tongkat Ali and the aqueous solution is 1:1 to 30, and the mixture is continuously ultrasonically extracted for 5 min to 5 h, and the ultrasonic extraction temperature is 10 to 70 °C.
- the supernatant is enriched with macroporous resin, and the resin type is preferably HP-20, D101, DM130, AB-8.
- the macroporous resin column is eluted with a gradient of one or several solvents in ethanol, ethyl acetate, and water.
- the eluate containing the target component of the ligninin (relanone) was collected, concentrated under reduced pressure, and precipitated twice with absolute ethanol to remove the impurities, and finally the active ingredient group A of Tongkat Ali was obtained.
- the effluent after adsorption of the macroporous resin is separated by a membrane filtration method, and the components of the Tongkat Ali water-soluble active polysaccharide, glycopeptide and amino acid are separated, sprayed or freeze-dried to obtain the active ingredient group B of Tongkat Ali.
- Tongkat Ali active ingredient group A and Tongkat Ali active ingredient group B were mixed in proportion to form Tongkat Ali active ingredient combination.
- the Tongkat Ali active ingredient combination prepared by the method has a plurality of components coexisting, the characteristic substance bitter lignin component content is 1 to 50%, and the content of various active polysaccharides, glycopeptides, amino acids and the like is 1 to 20%.
- the Tongkat Ali active ingredient combination prepared by the invention has the functions of enhancing sexual function, improving fertility, refreshing anti-fatigue, enhancing immunity, enhancing physical fitness and relieving gout.
- the extraction temperature is first controlled between 10 and 70 ° C, and the auxiliary ultrasonic extraction method can retain the activity of the two types of material components.
- the prepared Tongkat Ali active ingredient combination process is simple, the production process is safe and environmentally friendly, and the extraction rate and yield of the active ingredients are high, which is suitable for large-scale production.
- the active ingredients of different parts of Tongkat Ali are proposed.
- the mixed use method is used to prepare a combination of active ingredients of Tongkat Ali to enhance the overall effect of the drug.
- the production of Tongkat Ali active ingredient combination has been verified by many experiments, which has the functions of enhancing sexual function, improving fertility, refreshing anti-fatigue, enhancing immunity, enhancing physical fitness and relieving gout. It can be applied to the decline of non-organic sexual function in males. People with mental stress, fatigue, and the elderly with menopausal syndrome.
- Tongkat Aligen Take 100.0 g of Tongkat Aligen and immerse it in 2 L of distilled water.
- the water temperature is controlled at 50 °C.
- the pulverized Tongkat Ali was mixed with water and subjected to continuous ultrasonic extraction for 2 hours, and then filtered and centrifuged to obtain Tongkat Ali water extract.
- the water extract of Tongkat Ali was directly adsorbed to saturation by D101 resin, and the adsorption column was eluted with an aqueous solution of ethanol to collect the target components of the lignin, and the ethanol water eluate was obtained, and concentrated under reduced pressure to obtain the crude Tongkat Ali. 4.4 grams.
- the crude Tongkat Ali was dissolved in absolute ethanol, and the resulting precipitate was removed by suction filtration to obtain an ethanol solution of Tongkat Ali active ingredient, which was concentrated under reduced pressure to further obtain Tongkat Ali active ingredient group A.
- the effluent liquid is filtered by a membrane device, separated by a microfiltration membrane, an ultrafiltration membrane, a nanofiltration membrane, etc., and the nanofiltration membrane and the ultrafiltration membrane entrapment component are collected, and the active polysaccharide, the glycopeptide and the amino acid are separated, and finally Obtained 1.2 g of Tongkat Ali active ingredient group B.
- the Tongkat Ali active ingredient groups A and B were mixed in a ratio of 2:1 to prepare a Tongkat Ali active ingredient combination.
- the Tongkat Ali active ingredient combination was administered to ICR mice by intraperitoneal administration, and the experiment obtained the approximate lethal dose and the maximum non-toxic dose.
- the approximate lethal dose range for male mice is 100.0-120.0 mg/kg, and the maximum non-toxic dose is 80 mg/kg; the approximate lethal dose range for female mice is 180.0-225.0 mg/kg, and the maximum non-toxic dose is 80 mg/kg.
- the dead animals were dissected, and no abnormal pathological changes were observed in the main internal organs by naked eyes.
- the Tongkat Ali active ingredient combination was administered to ICR mice by intragastric administration, and the results showed that no toxicity was observed in the mice when the drug was administered at 500 mg/kg.
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
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Abstract
一种东革阿里有效成分的制备方法及其用途，所述制备方法包括下列步骤：在一定温度下，通过逆流超声提取东革阿里获得水提取液，用大孔树脂吸附、洗脱、醇沉后得到A组分；使用滤膜分级分离大孔树脂流出部分得到B组分；按一定比例混合A组分和B组分。所述东革阿里有效成分可增强性功能、提高生育率、提神抗疲劳、增强免疫力、增加体能、缓解痛风。
Description
本发明属于植物天然产物提取领域，具体涉及制备东革阿里植物有效成分及组合应用的方法。
背景介绍
东革阿里(Eurycoma longifolia)为苦木科东革阿里属植物，野生灌木，生长于赤道附近原始热带雨林潮湿砂质土壤中，在马来西亚、印度尼西亚、越南等东南亚同家分布较广。现代研究表明，东革阿里具有很高的药用价值。东革阿里植物根据各种不同处理方式获得的组分分别具有抗癌活性，抗疟活性，改善性功能等作用。除此之外，其在降血糖、抗菌、治疗痛风、骨质疏松等方面也有一定的效果。从东革阿里不同部位中分离出来的化学成分以含苦木素骨架的二萜类与铁屎米酮类生物碱为主，如eurycomaoside，eurycolactone，eurycomalactone，eurycomanone(宽缨酮)和pasakbumin-B。此外，还含有联苯木质素、角鲨烯衍生物、活性多糖、糖肽和多种氨基酸。目前，经过我们的研究发现，印尼引进的东革阿里采用本方法提取获得的有效成分组合具有增强性功能、提高生育率、提神抗疲劳、增强免疫力、增加体能、缓解痛风的作用。
东革阿里植物直接作为饮片使用的情况较为普遍，但是东革阿里冲泡存在口感苦涩、药效作用低和药物利用率低等方面的问题。因此，研究东革阿里有效成分含量高，制备工艺可靠、药用效果明确、口感良好的产品就变得十分重要。研究资料显示，东革阿里提取主要采用溶剂回流提取或高温水提取过程，如专利CN104757424A采用煎煮法提取；专利US20070224300A1采用沸水提取；“东革阿里对运动训练大鼠睾酮含量、物质代谢及抗运动疲劳能力的影响”文章采用沸水制备；“东革阿里化学成分的分离与鉴定”文章采用水回流提取。专利CN103408564A将东革阿里以有机溶剂提取；“东革阿里提取物抗疲劳作用的实验研究”文章使用醇提取工艺。以上两种方式虽然提取产物量相对较多，但是沸水提取和有机溶剂提取方式会使植物当中的多种活性成分分解或变性，降低了药物作用效果，同时能源消耗多，环保难度高，溶剂成本大，提取过程危害性强。
多方面的研究结果表明，东革阿里植物确实具有明显的增强性功能、提高生育率、提神抗疲劳、增强免疫力、增强体能、缓解痛风的作用，以各种不同方式获得的提取物普遍具有一定的增强活力效果，但其中的化学单一组分始终没有完全确认。综合多方面的文章报道和自身研究数据，我们发现以宽缨酮为代表的苦木素类物质和以活性多糖、糖肽和氨基酸类为
主的水溶性生物活性成分是其中的主要有效成分。我们根据研究和实践证实，这两部分有效成分共同使用具有一定的协同增效作用。
发明内容
本发明提供具有增强性功能、提高生育率、提神抗疲劳、增强免疫力、增加体能、缓解痛风的东革阿里有效成分组合制备方法。本方法不仅使用超声水溶液提取有效成分而且选用大孔树脂进行吸附分离和膜分离，保留了东革阿里植物中有效成分的生物活性并选择性地将其富集。
本发明提及的东革阿里有效成分其制备方法如下：
具有增强性功能、提高生育率、提神抗疲劳、增强免疫力、增强体能、缓解痛风的东革阿里有效成分组合制备方法，将东革阿里粉碎后与水溶液混合，经过连续逆流超声水提取处理，获得东革阿里水提取液；
a.水提取液过滤离心去除沉淀后直接经过大孔树脂吸附，吸附后树脂柱经洗脱液洗脱并收集目标组分，乙醇沉淀去除杂质，浓缩干燥，获得东革阿里有效成分组A；
b.水提取液经大孔树脂吸附后的流出液，采用滤膜分级分离，收集目标组分，减压浓缩、冷冻干燥或喷雾干燥，获得东革阿里有效成分组B；
c.按照一定比例，混合东革阿里有效成分组A和B，制成东革阿里有效成分组合。
具体为东革阿里与水溶液的质量体积比为1∶1～30，混合物连续超声提取5min～5h，超声提取温度为10～70℃。东革阿里超声水提取液过滤离心后，上清液用大孔树脂富集，树脂类型优选HP-20、D101、DM130、AB-8。吸附后大孔树脂柱采用乙醇、乙酸乙酯、水中的一种或几种溶剂混合梯度洗脱。收集含有苦木素类目标成分(宽缨酮)的洗脱液，减压浓缩，无水乙醇沉淀2次去除杂质，最终制得东革阿里有效成分组A。大孔树脂吸附后的流出液经，采用膜过滤方法，分离东革阿里水溶活性多糖、糖肽和氨基酸等组分，喷雾或冷冻干燥，获得东革阿里有效成分组B。东革阿里有效成分组A与东革阿里有效成分组B按照比例混合，形成东革阿里有效成分组合。本方法制得的东革阿里有效成分组合中多种成分共存，特征物质苦木素类成分含量在1～50％，多种活性多糖、糖肽、氨基酸等营养成分含量在1～20％。本发明制备的东革阿里有效成分组合具有增强性功能、提高生育率、提神抗疲劳、增强免疫力、增强体能、缓解痛风的作用。
采用本发明新的工艺技术首先控制提取温度在10～70℃之间，辅助超声提取方法，能够保留两类物质组分的活性。制备的东革阿里有效成分组合工艺流程简便、生产过程安全、环保，有效成分提取率、产率均高，适合大规模生产。其次提出将东革阿里不同部位有效成分
混合使用的方法制备东革阿里有效成分组合，增强整体的药物作用效果。生产的东革阿里有效成分组合经过多方面实验验证，具有增强性功能、提高生育率、提神抗疲劳、增强免疫力、增强体能、缓解痛风的作用，可以应用于男性非器质性性功能下降、精神压力大、容易疲劳等人群以及更年期综合症的老年人。
在下面的具体实施方案中进一步说明了本发明，这并不限制本发明的范围。在不脱离本发明上述技术思想情况下，根据本领域普通技术知识和惯用手段，做出各种替换和变更，均应包括在本发明的范围内。
1.制备方法
取东革阿里根100.0克粉碎，加入蒸馏水2L浸泡，水温控制在50℃。利用超声提取设备，将粉碎的东革阿里与水混合并进行连续超声提取2小时，再经过过滤、离心，获得东革阿里水提取液。东革阿里的水提取液直接使用D101树脂循环吸附至饱和，用乙醇水溶液对吸附柱进行洗脱，收集苦木素类目标成分，获得乙醇水洗脱液，减压浓缩，获得东革阿里粗品4.4克。东革阿里粗品用无水乙醇溶解，抽滤去除产生的沉淀，得到东革阿里有效成分乙醇溶液，减压浓缩，进一步获得东革阿里有效成分组A。大孔树脂吸附后流出液体采用膜设备过滤，经过微滤膜、超滤膜、纳滤膜等分离，收集纳滤膜和超滤膜截留成分，分离其中的活性多糖、糖肽和氨基酸，最终获得1.2g东革阿里有效成分组B。按照2∶1的比例混合东革阿里有效成分组A和B，制备成东革阿里有效成分组合。
2.小鼠急性毒性实验
将东革阿里有效成分组合按照腹腔注射给药方式给予ICR小鼠，实验获得近似致死剂量、最大无毒性剂量。雄性小鼠近似致死剂量范围为100.0-120.0mg/kg，最大无毒性剂量为80mg/kg；雌性小鼠近似致死剂量范围为180.0-225.0mg/kg，最大无毒性剂量为80mg/kg。对死亡动物进行解剖，肉眼观察主要内脏器官未见异常病理变化。
将东革阿里有效成分组合按照灌胃给药方式给予ICR小鼠，结果表明给药500mg/kg，小鼠未发现毒性表现。
Claims (9)
- 制备东革阿里(又名东哥阿里)有效成分组合的方法，其过程为：将东革阿里粉碎后与水溶液混合，在一定温度下，经过连续逆流超声水提取处理，获得东革阿里水提取液；a.水提取液过滤离心去除沉淀后直接经过大孔树脂吸附，吸附后树脂柱洗脱液洗脱并收集目标组分，乙醇沉淀去除杂质，清液浓缩干燥，获得东革阿里有效成分组A；b.水提取液经大孔树脂吸附后的流出液，采用滤膜分级分离，收集目标组分，减压浓缩、干燥，获得东革阿里有效成分组B；c.按照一定比例，混合东革阿里有效成分组A和B，制成东革阿里有效成分组合。
- 根据权利要求1所述东革阿里有效成分组合的制备方法，其原料为东革阿里(Eurycoma longifolia)，优选东革阿里树根。
- 根据权利要求1所述东革阿里有效成分组合的制备方法，其超声水溶液提取特征为东革阿里粉碎后与水溶液按照质量体积比为1∶1～30混合，混合液经过连续逆流超声提取，时间为5min～5h，超声提取控制温度为10～70℃。
- 根据权利要求1所述东革阿里有效成分组合的制备方法，其富集特征在于水提取液用大孔树脂吸附富集，树脂类型优选HP-20、D101、DM130、AB-8。
- 根据权利要求1所述东革阿里有效成分组合的制备方法，其树脂柱吸附成分洗脱特征在于树脂柱采用乙醇、乙酸乙酯、水中的一种或几种溶剂混合梯度洗脱。
- 根据权利要求1所述东革阿里有效成分组合的制备方法，其滤膜分级分离选择微滤膜、超滤膜、反渗透膜和钠滤膜一种或几种梯度处理。
- 根据权利要求1所述东革阿里有效成分组合的制备方法，其东革阿里有效成分组A主要为苦木素类物质，优选宽缨酮，含量在1～35％。
- 根据权利要求1所述东革阿里有效成分组合的制备方法，其东革阿里有效成分组B主要为活性多糖、糖肽和氨基酸。
- 根据权利要求1所述东革阿里有效成分组合的制备方法，其特征在于按照本方法获得的东革阿里有效成分组合具有增强性功能、提高生育率、提神抗疲劳、增强免疫力、增加体能、缓解痛风的作用。
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