CN102241659A - Purification method of alpha-mangostin - Google Patents
Purification method of alpha-mangostin Download PDFInfo
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- CN102241659A CN102241659A CN2011101175372A CN201110117537A CN102241659A CN 102241659 A CN102241659 A CN 102241659A CN 2011101175372 A CN2011101175372 A CN 2011101175372A CN 201110117537 A CN201110117537 A CN 201110117537A CN 102241659 A CN102241659 A CN 102241659A
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Abstract
The invention belongs to the field of natural product isolation and relates to a purification method of alpha-mangostin. The purification method comprises the following steps: 1) crushing mangosteen shells, adding 3-10 times of a 60-80% ethanol solution to soak and extract for 2-3 times, concentrating the extract while depressurizing, adding the concentrated solution into an aqueous two-phase solvent system for extraction, collecting the organic phase, and concentrating the collected organic phase to obtain a concentrate; 2) adding water to the concentrate for dispersion, adding the dispersed concentrate to a polyamide column for adsorption, carrying out gradient elution with an ethanol solution, detecting by thin-layer chromatography, collecting the eluate, concentrating the eluate while depressurizing, and standing for crystallization; and 3) filtering out the crystals, dissolving the crystals with a mixed solution, recrystallizing, and drying to obtain alpha-mangostin. The purification method of alpha-mangostin is simple in process and easy to operate, has high product purity, and is easy to enlarge production.
Description
Technical field:
The invention belongs to the Separation of Natural Products field, relate to a kind of method of purifying α-mangostin.
Background technology:
α-mangostin (α-mangostin, α-MAG), be commonly called as α-mangosteen flavones, chemical name 1,3,6-trihydroxy--7-methoxyl group-2,8 pair (3-methyl-2-butene)-9-mouth mountain ketone, molecular formula C
24H
26O
6, molecular weight 410.47, molecular structural formula:
Mangosteen belongs to the fruit of garcinia plant, cries mangosteen, mangosteen, garcinia mangostana again, is a kind of tropical fruit, mangosteen shell treatment dysentery, malaria, sprain, typhoid fever, ulcer, skin infections, anti-inflammation and sterilization and help the folk tradition medication of wound healing.Wherein effective constituent α-mangostin has antibiotic, anti-inflammatory, the effect of anti-oxidant, anticancer and anti-AIDS, enjoys people to pay close attention in recent years.
Existing extraction separation α-mangostin method is many with adopting extraction using alcohol → chloroform or ethyl acetate extraction → silicagel column to separate.Patent (patent No. CN101525328) " is extracted the method for α-mangostin " from peel of Carcinia mangostana L., the method for this patent disclosure is: (I) extract; (II) concentrate: above-mentioned each extracting solution is merged, and concentrating under reduced pressure gets concentrated solution; (III) ethyl acetate extraction; (IV) silica gel column chromatography; (V) coarse crystallization; (VI) recrystallization.(patent No.: 201010181155) " a kind of preparation method of mangostin ", the method for this patent disclosure is patent: get the Garcinia Bark shell, pulverize, join CO
2In the supercritical extraction device, ethanol gets extract as entrainment agent, is added on the polymeric amide chromatography post, with volume ratio be 8: 1 methylene chloride-methanol mixed solvent as the eluent wash-out, reclaim solvent, crystallization, fractional crystallization, with the toluene recrystallization, fractional crystallization washs, is drying to obtain.The extracting method of crude extract adopts macroporous resin purification, in addition as document " polymeric adsorbent is to mangosteen chromocor compound Study on adsorption property ".As mentioned above, there are two kinds of problems in the method for existing purifying α-mangostin: the one, and content height but complex process; The 2nd, technology is simple but content is low.
Summary of the invention
The objective of the invention is provides a kind of method of purifying α-mangostin in order to overcome the deficiencies in the prior art, and technological operation is simple, products obtained therefrom content height.
The technology of the present invention solution is as follows:
A kind of method of purifying α-mangostin is characterized in that may further comprise the steps:
1) get the mangosteen shell and pulverize, add 3-10 and doubly measure 60-80% alcohol solution dipping extraction 2-3 time, extracting solution concentrating under reduced pressure, concentrated solution add the extraction of double water-phase solvent systems, collect organic phase and concentrate, and get concentrated solution;
2) concentrated solution adds water-dispersion, adds polyamide column absorption, the ethanolic soln gradient elution, and thin layer detects, and collects the flow point concentrating under reduced pressure, places crystallization;
3) crystallisate leaches and uses the mixing solutions dissolving-recrystallization, is drying to obtain α-mangostin.
Double water-phase solvent systems in the described step 1) is ethanol, water, ammonium sulfate, blending ratio 4: 5: 5.
Described step 2) the ethanolic soln gradient elution that adopts in is: 4-5 doubly measures 20-30% ethanolic soln → 4-6 and doubly measures the 50-70% ethanolic soln.
The mixing solutions that adopts in the described step 3) is: sherwood oil, ethyl acetate, methyl alcohol, water, ratio of mixture (3-4): (5-6): 5: 3, get phase.
Technical superiority of the present invention is to adopt aqueous two-phase extraction to substitute the extraction of toxicity organic reagent, operational safety, environmental protection; Polymeric amide separates and mixing solutions crystallization substituted for silicon plastic column chromatography, makes technology be easy to reappear and amplification, has realized the industrialization of high content of alpha-mangostin product, for carry out α-mangostin more extensive use lay a good foundation.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
Get the mangosteen shell and pulverize, weighing 10kg adds 10 times of amount 80% ethanolic solns and is heated to 60 ℃, soaks 2 hours, and filtered solution adds 3 times of amount 80% ethanol again and is heated to 60 ℃ of extractions 2 hours, extracts 2 times, and the merging filtrate concentrating under reduced pressure gets concentrated solution.Get ethanol, water, ammonium sulfate, mix at 4: 5: 5 in proportion, it is centrifugal to add the concentrated solution tubular type, collects organic phase and concentrates, and concentrated solution adds water-dispersion, add the absorption of 2L polyamide column, use 8L30% ethanolic soln → 12L50% ethanolic soln wash-out successively, thin layer detects, and collects the high density flow point, concentrating under reduced pressure is placed crystallization.Get sherwood oil, ethyl acetate, methyl alcohol, water, by 4: 6: 5: 3 mixed, get phase solution dissolving coarse crystallization, saturated dissolving refluxes, filter and place crystallization, recrystallization 2 times leaches the crystallisate drying, get yellow powder 213g, detect through high performance liquid phase, α-mangostin content is 92.4%.
Embodiment 2:
Get the mangosteen shell and pulverize, weighing 10kg adds 10 times of amount 60% ethanolic solns and is heated to 50 ℃, soaks 3 hours, extracts 2 times, and the merging filtrate concentrating under reduced pressure gets concentrated solution.Get ethanol, water, ammonium sulfate, mix at 4: 5: 5 in proportion, it is centrifugal to add the concentrated solution tubular type, collects organic phase and concentrates, and concentrated solution adds water-dispersion, add the absorption of 2L polyamide column, use 10L20% ethanolic soln → 8L70% ethanolic soln wash-out successively, thin layer detects, and collects the high density flow point, concentrating under reduced pressure is placed crystallization.Get sherwood oil, ethyl acetate, methyl alcohol, water, by 3: 5: 5: 3 mixed, get phase solution dissolving coarse crystallization, saturated dissolving refluxes, filter and place crystallization, recrystallization 3 times leaches the crystallisate drying, get yellow powder 232g, detect through high performance liquid phase, α-mangostin content is 95.3%.
Embodiment 3:
Get the mangosteen shell and pulverize, weighing 10kg adds 8 times of amount 70% ethanolic solns and is heated to 50 ℃, soaks 3 hours, extracts 2 times, and the merging filtrate concentrating under reduced pressure gets concentrated solution.Get ethanol, water, ammonium sulfate, mix at 4: 5: 5 in proportion, it is centrifugal to add the concentrated solution tubular type, collects organic phase and concentrates, and concentrated solution adds water-dispersion, add the absorption of 2L polyamide column, use 10L30% ethanolic soln → 9L60% ethanolic soln wash-out successively, thin layer detects, and collects the high density flow point, concentrating under reduced pressure is placed crystallization.Get sherwood oil, ethyl acetate, methyl alcohol, water, by 3: 6: 5: 3 mixed, get phase solution dissolving coarse crystallization, saturated dissolving refluxes, filter and place crystallization, recrystallization 2 times leaches the crystallisate drying, get yellow powder 218g, detect through high performance liquid phase, α-mangostin content is 96.1%.
Embodiment 4:
Get the mangosteen shell and pulverize, weighing 50kg adds 8 times of amount 70% ethanolic solns and is heated to 50 ℃, soaks 3 hours, extracts 2 times, and the merging filtrate concentrating under reduced pressure gets concentrated solution.Get ethanol, water, ammonium sulfate, mix at 4: 5: 5 in proportion, it is centrifugal to add the concentrated solution tubular type, collects organic phase and concentrates, and concentrated solution adds water-dispersion, add the absorption of 10L polyamide column, use 50L30% ethanolic soln → 50L60% ethanolic soln wash-out successively, thin layer detects, and collects the high density flow point, concentrating under reduced pressure is placed crystallization.Get sherwood oil, ethyl acetate, methyl alcohol, water, by 3: 6: 5: 3 mixed, get phase solution dissolving coarse crystallization, saturated dissolving refluxes, filter and place crystallization, recrystallization 2 times leaches the crystallisate drying, get yellow powder 1103g, detect through high performance liquid phase, α-mangostin content is 93.4%.
Claims (4)
1. the method for a purifying α-mangostin is characterized in that may further comprise the steps:
1) get the mangosteen shell and pulverize, add 3-10 and doubly measure 60-80% alcohol solution dipping extraction 2-3 time, extracting solution concentrating under reduced pressure, concentrated solution add the extraction of double water-phase solvent systems, collect organic phase and concentrate, and get concentrated solution;
2) concentrated solution adds water-dispersion, adds polyamide column absorption, the ethanolic soln gradient elution, and thin layer detects, and collects the flow point concentrating under reduced pressure, places crystallization;
3) crystallisate leaches and uses the mixing solutions dissolving-recrystallization, is drying to obtain α-mangostin.
2. according to the method for the described purifying α-mangostin of claim 1, it is characterized in that the double water-phase solvent systems in the described step 1) is ethanol, water, ammonium sulfate, blending ratio 4: 5: 5.
3. according to the method for the described purifying α-mangostin of claim 1, it is characterized in that described step 2) in the ethanolic soln gradient elution be: 4-5 doubly measures 20-30% ethanolic soln → 4-6 and doubly measures the 50-70% ethanolic soln.
4. according to the method for the described purifying α-mangostin of claim 1, it is characterized in that the mixing solutions in the described step 3) is: sherwood oil, ethyl acetate, methyl alcohol, water, ratio of mixture (3-4): (5-6): 5: 3, get phase.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618071A (en) * | 2012-03-08 | 2012-08-01 | 桂林理工大学 | Method for extracting garcinia mangostana pericarp pigment by ultrasonic wave method |
| CN103467433A (en) * | 2013-09-30 | 2013-12-25 | 桂林茗兴生物科技有限公司 | Method for extracting alpha-mangostin from garcinia mangostana peel |
| CN103880807A (en) * | 2014-03-18 | 2014-06-25 | 杭州博麦医药科技有限公司 | Synthesis process of high-purity alpha-mangostin |
| CN104892561A (en) * | 2015-06-08 | 2015-09-09 | 桂林莱茵生物科技股份有限公司 | Method for extracting high-content alpha-mangostin from mangosteen skin |
| CN105130945A (en) * | 2015-08-30 | 2015-12-09 | 常州市鼎日环保科技有限公司 | Method for separating and purifying alpha-mangostin from garcinia mangostana |
| CN107382950A (en) * | 2017-07-27 | 2017-11-24 | 上海中医药大学 | GaroliganthoneC and its pharmaceutical composition and purposes |
| CN111170981A (en) * | 2020-01-21 | 2020-05-19 | 浙江省人民医院 | Garcinia extract extracted from mangosteen, preparation method and application thereof |
| CN114392214A (en) * | 2021-12-24 | 2022-04-26 | 赤峰福纳康生物技术有限公司 | Extraction method and application of mangosteen effective part |
| US11517601B2 (en) | 2020-07-21 | 2022-12-06 | Junhong Biotechnology Co., Ltd. | Mangosteen pericarp extract and process for its preparation thereof |
-
2011
- 2011-05-06 CN CN2011101175372A patent/CN102241659A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618071A (en) * | 2012-03-08 | 2012-08-01 | 桂林理工大学 | Method for extracting garcinia mangostana pericarp pigment by ultrasonic wave method |
| CN103467433A (en) * | 2013-09-30 | 2013-12-25 | 桂林茗兴生物科技有限公司 | Method for extracting alpha-mangostin from garcinia mangostana peel |
| CN103880807B (en) * | 2014-03-18 | 2016-09-28 | 杭州博麦医药科技有限公司 | The synthesis technique of high-purity alpha-mangostin |
| CN103880807A (en) * | 2014-03-18 | 2014-06-25 | 杭州博麦医药科技有限公司 | Synthesis process of high-purity alpha-mangostin |
| CN104892561B (en) * | 2015-06-08 | 2017-06-16 | 桂林莱茵生物科技股份有限公司 | A kind of method that high content of alpha mangostin is extracted from mangosteen skin |
| CN104892561A (en) * | 2015-06-08 | 2015-09-09 | 桂林莱茵生物科技股份有限公司 | Method for extracting high-content alpha-mangostin from mangosteen skin |
| CN105130945A (en) * | 2015-08-30 | 2015-12-09 | 常州市鼎日环保科技有限公司 | Method for separating and purifying alpha-mangostin from garcinia mangostana |
| CN107382950A (en) * | 2017-07-27 | 2017-11-24 | 上海中医药大学 | GaroliganthoneC and its pharmaceutical composition and purposes |
| CN107382950B (en) * | 2017-07-27 | 2019-10-15 | 上海中医药大学 | Garoliganthone C and its pharmaceutical composition and purposes |
| CN111170981A (en) * | 2020-01-21 | 2020-05-19 | 浙江省人民医院 | Garcinia extract extracted from mangosteen, preparation method and application thereof |
| CN111170981B (en) * | 2020-01-21 | 2022-04-19 | 浙江省人民医院 | Garcinia extract extracted from mangosteen, preparation method and application thereof |
| US11517601B2 (en) | 2020-07-21 | 2022-12-06 | Junhong Biotechnology Co., Ltd. | Mangosteen pericarp extract and process for its preparation thereof |
| TWI789606B (en) * | 2020-07-21 | 2023-01-11 | 潤鴻生物科技股份有限公司 | Mangosteen husk extract and preparation method thereof |
| CN114392214A (en) * | 2021-12-24 | 2022-04-26 | 赤峰福纳康生物技术有限公司 | Extraction method and application of mangosteen effective part |
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Application publication date: 20111116 |