CN104558067A - Method for extracting and separating syringin from medicinal material of ovateleaf holly bark - Google Patents
Method for extracting and separating syringin from medicinal material of ovateleaf holly bark Download PDFInfo
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- CN104558067A CN104558067A CN201410835321.3A CN201410835321A CN104558067A CN 104558067 A CN104558067 A CN 104558067A CN 201410835321 A CN201410835321 A CN 201410835321A CN 104558067 A CN104558067 A CN 104558067A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/203—Monocyclic carbocyclic rings other than cyclohexane rings; Bicyclic carbocyclic ring systems
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
Abstract
The invention discloses a method for extracting and separating syringin from a medicinal material of ovateleaf holly bark. The method comprises the following operation steps: (1) crushing the medicinal material of ovateleaf holly bark, allowing the crushed ovateleaf holly bark to pass a 20-50-mesh sieve, adding water for extraction, and performing centrifugal concentration on extract to obtain upper column liquid; (2) allowing the upper column liquid to pass through a resin column, performing elution with water and 10-40% ethanol (v/v) respectively, and sectionally collecting eluent; (3) performing membrane separation concentration and spray-drying on the part eluted with 10-40% ethanol (v/v) ethanol to obtain the product. The method is simple in process, high in operability, low in cost and suitable for industrial production.
Description
Technical field
The invention belongs to active pharmaceutical ingredients extraction and separation technology field, specifically, relate to the extracting and developing method of Syringin in Ilex rotunda Thunb. medicinal material.
Background technology
Ilex rotunda Thunb. is bark or the root skin of Ilex rotunda Thunb., main product in Jiangsu, Anhui, Jiangxi, Fujian, Guangdong, the area such as Guangxi, for south China, people side commonly uses herbal medicine.Have clearing heat and detoxicating, effect of dampness removing pain relieving, be usually used in the heating for the treatment of summer-heat and damp, swelling and pain in the throat, damp-heat dysentery, abdominal distention, rheumatic arthralgia, condyloma, sore furuncle, wound etc.Syringin is syringin again, is the main component in Ilex rotunda Thunb. activeconstituents, has anti-inflammatory, analgesia and antitumor action, can be used for hemostasis and anti-liver poison.
The method of published extraction and isolation Syringin from Ilex rotunda Thunb. medicinal material is few at present, patent CN 1010724 A discloses the technique of method extraction purification Syringin of water extract-alcohol precipitation, the dry silica gel stirring of medicinal extract, organic solvent extraction, crystallization, unit operation is too much, long, and discontinuous, be unfavorable for suitability for industrialized production; The method that patent CN 10103534 A discloses alcohol extracting-water precipitating, iron holly bark total saponins is prepared in centrifuging, product total saponin content only reaches 50%, is difficult to meet the demand developing more high purity product; Patent CN 101307079 A discloses benzene refluxing extraction, the method for the extraction of dregs of a decoction acetone reflux, repeatedly recrystallization extracts Syringin, and in process, consumption of organic solvent is too much, and environmental pollution is larger; Patent CN 102070684 A discloses water extraction, concentrated solution adds activated carbon decolorizing, filter under solution acidic condition, prepare the method for Syringin under solution neutral condition with n-butanol extraction, reclaim under reduced pressure n-butanol extraction, this technique consumption of organic solvent is many, and repeatedly concentrate, energy consumption is large, is unfavorable for suitability for industrialized production.
Instant invention overcomes the shortcomings such as consumption of organic solvent in traditional technology is large, the production cycle is long, energy consumption is high, adopt water extraction-macroporous resin adsorption be separated-efficient nanofiltration membrane concentrates-spray-dired technique realizes the preparation of Syringin and successfully realize industrialization.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of simple, strong operability, efficient, energy consumption is low, be applicable to the method for extraction and isolation Syringin from Ilex rotunda Thunb. medicinal material of suitability for industrialized production.
Technical scheme of the present invention is as follows:
(1) Ilex rotunda Thunb. pulverizing medicinal materials to 20 ~ 50 order, extracting in water 1 ~ 3 time, each 60 ~ 180 min, united extraction liquid, is evaporated to density 1.01 ~ 1.20 g/ml and obtains upper prop liquid;
(2) upper prop liquid is entered macroporous resin column, washed resin is closely colourless to effluent liquid, then uses 10 ~ 40% ethanol (v/v) wash-out, collects elutriant, and eluent through nanofiltration membrane is concentrated into total solid content 25 ~ 35% and obtains concentrated solution;
(3) concentrated solution is spray-dried obtains product.
In above-mentioned preparation method:
In step (1), the consumption of water is 5 ~ 20 times of raw material weight, preferably 8 ~ 10 times.
In step (2), described macroporous resin is nonpolar or low-pole macroporous resin, and preferred model is AB-8, HPD100, D101, D130, SP825 or HP20.
In step (2), the consumption of water is 2 ~ 6 times of resin column volume, and the consumption of 10 ~ 40% ethanol (v/v) is 2 ~ 7 times of resin column volume.
In step (2), described membrane separation concentration technique, film used is polymeric amide high temperature nanofiltration membrane.
In step (3), in described drying process with atomizing, inlet temperature 170 ~ 210 DEG C, temperature of charge 70 DEG C, air outlet temperature 90 ~ 120 DEG C.
Simmer down to employing described in aforesaid method is existing prepares operation identical in Syringin method.
The present invention for starting raw material with Ilex rotunda Thunb. medicinal material, adopts water extraction-macroporous resin adsorption separation-nanofiltration membrane to concentrate-spray-dired operational path, realizes the preparation of Syringin.Tool of the present invention has the following advantages:
1, with water level Extraction solvent, cost is low, environmentally safe;
2, take macroporous resin as sorbent material, aqueous ethanolic solution gradient elution, solvent, resin recoverable;
3, by membrane separation concentration technique, reduce energy consumption, reduce production cost;
3, technological process is simple, workable, is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of extraction and isolation Syringin from Ilex rotunda Thunb. medicinal material.
Embodiment
embodiment 1:
After Ilex rotunda Thunb. pulverizing medicinal materials, cross 20 mesh sieves, claim 220kg to be placed in 3 tons of extractors, add 100 DEG C, the water extraction of 10 times of raw material weights, first time extracts 120min, leaches liquid, then adds the water of 8 times of raw material weights, refluxing extraction 60min, united extraction liquid;
Extracting solution is evaporated to density 1.01 g/ml and obtains upper prop liquid; Enter AB-8 macroporous resin column, be washed to elutriant closely colourless, then use 4 column volume 20% ethanol (v/v) wash-outs, collect 20% ethanol (v/v) elutriant, membrane separation concentrated be reduced to solid content 30% after, spray-dried product 0.95kg.
According to the content assaying method of 2010 editions pharmacopeia Syringins, through HPLC analyzing and testing, Syringin purity is 78.56%.
embodiment 2:
After Ilex rotunda Thunb. pulverizing medicinal materials, cross 20 mesh sieves, claim 220kg to be placed in 3 tons of extractors, add 100 DEG C, the water extraction of 10 times of raw material weights, first time extracts 180min, leaches liquid, then adds the water of 8 times of raw material weights, refluxing extraction 90min, united extraction liquid;
Extracting solution is evaporated to density 1.05 g/ml and obtains upper prop liquid; Enter SP825 macroporous resin column, be washed to elutriant closely colourless, then use 3 column volume 20% ethanol (v/v) wash-outs, collect 20% ethanol (v/v) elutriant, membrane separation concentrated be reduced to solid content 25% after, spray-dried product 0.86kg.
According to the content assaying method of 2010 editions pharmacopeia Syringins, through HPLC analyzing and testing, Syringin purity is 83.34%.
embodiment 3
After Ilex rotunda Thunb. pulverizing medicinal materials, cross 30 mesh sieves, claim 200kg to be placed in 3 tons of extractors, add the micro-extraction of boiling of water of 9 times of raw material weights, first time extracts 120min, leaches liquid, then adds the water of 9 times of raw material weights, refluxing extraction 60min, united extraction liquid;
Extracting solution is evaporated to density 1.04 g/ml and obtains upper prop liquid; Enter HP20 macroporous resin column, be washed to elutriant closely colourless, then use 4 column volume 30% ethanol (v/v) wash-outs, collect 30% ethanol (v/v) elutriant, membrane separation concentrated be reduced to solid content 25% after, spray-dried product 0.87kg.
According to the content assaying method of 2010 editions pharmacopeia Syringins, through HPLC analyzing and testing, Syringin purity is 76.23%.
embodiment 4:
After Ilex rotunda Thunb. pulverizing medicinal materials, cross 50 mesh sieves, claim 200kg to be placed in 3 tons of extractors, add the micro-extraction of boiling of water of 10 times of raw material weights, first time extracts 120min, leaches liquid, then adds the water of 8 times of raw material weights, refluxing extraction 60min, united extraction liquid;
Extracting solution is evaporated to density 1.03 g/ml and obtains upper prop liquid; Enter HPD100 macroporous resin column, be washed to elutriant closely colourless, then use 3 column volume 15% ethanol (v/v) wash-outs, collect 15% ethanol (v/v) elutriant, membrane separation concentrated be reduced to solid content 30% after, spray-dried product 0.84kg.
According to the content assaying method of 2010 editions pharmacopeia Syringins, through HPLC analyzing and testing, Syringin purity is 85.27%.
embodiment 5:
After Ilex rotunda Thunb. pulverizing medicinal materials, cross 20 mesh sieves, claim 220kg to be placed in 3 tons of extractors, add 100 DEG C, the water extraction of 11 times of raw material weights, first time extracts 180min, leaches liquid, then adds the water of 9 times of raw material weights, refluxing extraction 90min, united extraction liquid;
Extracting solution is evaporated to density 1.03 g/ml and obtains upper prop liquid; Enter AB-8 macroporous resin column, be washed to elutriant closely colourless, then use 4 column volume 20% ethanol (v/v) wash-outs, collect 20% ethanol (v/v) elutriant, membrane separation concentrated be reduced to solid content 25% after, spray-dried product 1.01kg.
According to the content assaying method of 2010 editions pharmacopeia Syringins, through HPLC analyzing and testing, Syringin purity is 76.33%.
embodiment 6:
After Ilex rotunda Thunb. pulverizing medicinal materials, cross 20 mesh sieves, claim 220kg to be placed in 3 tons of extractors, add 100 DEG C, the water extraction of 9 times of raw material weights, first time extracts 120min, leaches liquid, then adds the water of 8 times of raw material weights, refluxing extraction 90min, united extraction liquid;
Extracting solution is evaporated to density 1.05 g/ml and obtains upper prop liquid; Enter SP825 macroporous resin column, be washed to elutriant closely colourless, then use 4 column volume 20% ethanol (v/v) wash-outs, collect 20% ethanol (v/v) elutriant, membrane separation concentrated be reduced to solid content 25% after, spray-dried product 0.93kg.
According to the content assaying method of 2010 editions pharmacopeia Syringins, through HPLC analyzing and testing, Syringin purity is 78.37%.
embodiment 7:
After Ilex rotunda Thunb. pulverizing medicinal materials, cross 30 mesh sieves, claim 200kg to be placed in 3 tons of extractors, add the micro-extraction of boiling of water of 9 times of raw material weights, first time extracts 180min, leaches liquid, then adds the water of 8 times of raw material weights, refluxing extraction 90min, united extraction liquid;
Extracting solution is evaporated to density 1.01 g/ml and obtains upper prop liquid; Enter HP20 macroporous resin column, be washed to elutriant closely colourless, then use 5 column volume 30% ethanol (v/v) wash-outs, collect 30% ethanol (v/v) elutriant, membrane separation concentrated be reduced to solid content 30% after, spray-dried product 0.83kg.
According to the content assaying method of 2010 editions pharmacopeia Syringins, through HPLC analyzing and testing, Syringin purity is 76.23%.
embodiment 8:
After Ilex rotunda Thunb. pulverizing medicinal materials, cross 50 mesh sieves, claim 200kg to be placed in 3 tons of extractors, add the micro-extraction of boiling of water of 10 times of raw material weights, first time extracts 180min, leaches liquid, then adds the water of 8 times of raw material weights, refluxing extraction 120min, united extraction liquid;
Extracting solution is evaporated to density 1.01 g/ml and obtains upper prop liquid; Enter HPD100 macroporous resin column, be washed to elutriant closely colourless, then use 4 column volume 15% ethanol (v/v) wash-outs, collect 15% ethanol (v/v) elutriant, membrane separation concentrated be reduced to solid content 30% after, spray-dried product 0.85kg.
According to the content assaying method of 2010 editions pharmacopeia Syringins, through HPLC analyzing and testing, Syringin purity is 85.27%.
Claims (7)
1. the method for extraction and isolation Syringin from Ilex rotunda Thunb. medicinal material, is characterized in that comprising the steps:
(1) Ilex rotunda Thunb. pulverizing medicinal materials to 20 ~ 50 order, extracting in water 1 ~ 3 time, each 60 ~ 180 min, united extraction liquid, is evaporated to density 1.01 ~ 1.20 g/ml and obtains upper prop liquid;
(2) upper prop liquid is entered macroporous resin column, washed resin is closely colourless to effluent liquid, then uses 10 ~ 40% ethanol (v/v) wash-out, collects elutriant, and eluent through nanofiltration membrane is concentrated into total solid content 25 ~ 35% and obtains concentrated solution;
(3) concentrated solution is spray-dried obtains product.
2. method according to claim 1, is characterized in that: in step (1), and the consumption of water is 5 ~ 20 times of raw material weight.
3. method according to claim 1, is characterized in that: in step (2), and described macroporous resin is nonpolar or low-pole macroporous resin.
4. method according to claim 3, is characterized in that: in step (2), and the model of described macroporous resin is AB-8, HPD100, D101, D130, SP825 or HP20.
5. method according to claim 1, is characterized in that: in step (2), and the consumption of water is 2 ~ 6 times of resin column volume, and the consumption of 10 ~ 40% ethanol (v/v) is 2 ~ 7 times of resin column volume.
6. method according to claim 1, is characterized in that: in step (2), described membrane separation concentration technique, and film used is polymeric amide high temperature nanofiltration membrane.
7. method according to claim 1, is characterized in that: in step (3), in described drying process with atomizing, inlet temperature 170 ~ 210 DEG C, temperature of charge 70 DEG C, air outlet temperature 90 ~ 120 DEG C.
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| CN201410835321.3A CN104558067B (en) | 2014-12-30 | 2014-12-30 | A kind of method that separating syringin is extracted in the medicinal material from iron holly bark |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101240004A (en) * | 2008-03-18 | 2008-08-13 | 山东大学威海分校 | Technique for preparing eleutheroside B |
| CN101643484A (en) * | 2008-08-06 | 2010-02-10 | 苑立超 | High-purity syringin, preparation method and application |
| CN102070684A (en) * | 2010-12-24 | 2011-05-25 | 南京泽朗医药科技有限公司 | Method for extracting syringin |
| CN102643322A (en) * | 2012-03-29 | 2012-08-22 | 中国中医科学院中药研究所 | Method for simultaneously preparing pedunculoside and syringin |
| CN103351419A (en) * | 2013-07-09 | 2013-10-16 | 陕西中药研究所 | Two-step simultaneous preparation method for pedunculoside and syringin |
-
2014
- 2014-12-30 CN CN201410835321.3A patent/CN104558067B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101240004A (en) * | 2008-03-18 | 2008-08-13 | 山东大学威海分校 | Technique for preparing eleutheroside B |
| CN101643484A (en) * | 2008-08-06 | 2010-02-10 | 苑立超 | High-purity syringin, preparation method and application |
| CN102070684A (en) * | 2010-12-24 | 2011-05-25 | 南京泽朗医药科技有限公司 | Method for extracting syringin |
| CN102643322A (en) * | 2012-03-29 | 2012-08-22 | 中国中医科学院中药研究所 | Method for simultaneously preparing pedunculoside and syringin |
| CN103351419A (en) * | 2013-07-09 | 2013-10-16 | 陕西中药研究所 | Two-step simultaneous preparation method for pedunculoside and syringin |
Non-Patent Citations (2)
| Title |
|---|
| 李津明: "《现代制药技术》", 30 April 2005, 中国医药科技出版社 * |
| 许锦涛，等: "富集纯化救必应总皂苷的大孔吸附树脂筛选", 《中国中医药现代远程教育》 * |
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