CN103933127A - Preparation method of forsythia total glycosides - Google Patents
Preparation method of forsythia total glycosides Download PDFInfo
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- CN103933127A CN103933127A CN201410149410.2A CN201410149410A CN103933127A CN 103933127 A CN103933127 A CN 103933127A CN 201410149410 A CN201410149410 A CN 201410149410A CN 103933127 A CN103933127 A CN 103933127A
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- fructus forsythiae
- extraction
- ethyl acetate
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- total glycosides
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Abstract
The invention relates to a preparation method of forsythia total glycosides. The preparation method comprises the following steps: A, percolation: smashing fructus forsythiae to 20-40 meshes, and percolating fructus forsythiae for 36-48 hours by a 40-70% low alcohol solution to obtain a percolate, and then, concentrating under reduced pressure at 55-65 DEG C, wherein the volume of the concentrated liquor is 1/5-1/4 of the percolate; B, extraction: preparing an organic solvent with less polarity and ethyl acetate in a volume ratio of 1:(0.5-1) to an extracting liquid, extracting for 2-4 times by the extracting liquor equivalent to the concentrated liquor in volume, and abandoning the extracting part to obtain a mother liquid; C, salting and extracting: adding strong acid weak base salt soluble in water into the mother liquid so that the pH is 3-5, then, extracting for 4-6 times by an ethyl acetate/methanol mixed liquid equivalent to the mother liquid in volume, combining the extract and concentrating under reduced pressure to be dry to obtain the forsythia total glycosides. The preparation method is simple to operate, low in cost and suitable for industrialized production. The forsythia total glycosides prepared are high in yield, high in content and good in pharmacodynamic action.
Description
Technical field
The present invention relates to a kind of preparation method of Fructus Forsythiae ester glycoside.
Background technology
Fructus Forsythiae (Forsythia suspense) is the dry fruit of Oleaceae plants Fructus Forsythiae, and main product is in China Shanxi, Henan, Shaanxi and other places.Fructus Forsythiae medical material has antipyretic, antiinflammatory, and antibacterial, antiviral, removing toxic substances protect the liver with town and the pharmacological effect effect such as tell.Its main effective ingredient is phillyrin and Fructus Forsythiae ester glycoside (forsythiaside) two constituents, and wherein Fructus Forsythiae ester glycoside comprises forsythiaside A, B, and C, D, E etc. are especially the highest with the content of forsythiaside A (forsythiaside A).
Because Fructus Forsythiae ester glycoside is phenethyl alcohol glycoside compounds, and in Herba Cistanches medical material, topmost bioactive substance is also phenethyl alcohol glycoside compounds.Therefore adopt certain process means enrichment Fructus Forsythiae ester glycoside, the Fructus Forsythiae total glycosides obtaining may be used to the famous and precious rare Chinese medicine-Herba Cistanches replacing in condition in imminent danger.
The preparation method of Fructus Forsythiae total glycosides mainly contains macroporous resin column, silicagel column, polyamide column at present.It is that the low-alcohol solution of 30%-60% carries out eluting that macroporous resin column chromatography needs water content, and Fructus Forsythiae ester glycoside is to thermo-responsive, non-refractory, moisture eluent needs the distilling under reduced pressure of long period, Fructus Forsythiae ester glycoside can decompose in this course, causes the content of Fructus Forsythiae ester glycoside of prepared product low.Silicagel column, polyamide column method need to be used a large amount of disposable fillers, and its consumption of materials is large, and cost is high, is unsuitable for suitability for industrialized production.
Summary of the invention
The object of this invention is to provide a kind of preparation method of Fructus Forsythiae total glycosides, this method easy and simple to handle, with low cost, be suitable for suitability for industrialized production, and its yield of Fructus Forsythiae total glycosides that makes thing is high, the content of Fructus Forsythiae ester glycoside is high, drug action is good.
It is that a kind of preparation method of Fructus Forsythiae total glycosides, comprises the steps: that the present invention realizes the technical scheme that its goal of the invention adopts
A: diafiltration
By Fructus Forsythiae pulverizing medicinal materials to 20-40 order, the low-alcohol solution that is 40%-70% by volume fraction carries out the diafiltration of 36-48h to Fructus Forsythiae medical material, percolate, percolate concentrating under reduced pressure at 55-65 DEG C of temperature obtains concentrated solution, the volume of concentrated solution is percolate 1/5～1/4;
B: extraction
Little polarity organic reagent and ethyl acetate are mixed with to extract by the volume ratio of 1:0.5～1, then with the concentrated solution extraction of extract equity volume 2-4 time, discard extraction part and obtain mother solution;
C: saline extraction
Mother solution in step B adds strong acid weak base salt soluble in water, adjusts mother solution pH to 3-5, then uses and the isopyknic ethyl acetate/methanol mixed liquor extraction of mother solution 4-6 time, and combining extraction liquid, is evaporated to dryly, obtains Fructus Forsythiae total glycosides.
Compared with prior art, useful achievement of the present invention is:
One, whole operation only needs diafiltration under liquid room temperature and the extraction of two steps, and technological operation is easy, without special equipment, and also, without using disposable filler, its material consumption is low, low, the applicable industrialization of preparation cost.
Two, water-free ethyl acetate/methanol mixed liquor (extract), the concentrating under reduced pressure time after extraction is short, the decomposition of little of Fructus Forsythiae ester glycoside, the yield of Fructus Forsythiae total glycosides that makes thing is high, and the content of Fructus Forsythiae ester glycoside is high, and drug action is good.Test shows, the mass content that the present invention makes the forsythiaside A of thing is all greater than 50%.
Fructus Forsythiae medical material in above-mentioned steps A is blue or green Fructus Forsythiae medical material.
In blue or green Fructus Forsythiae, the content of Fructus Forsythiae ester glycoside is higher, thereby ensures that the Fructus Forsythiae ester glycoside content of prepared product is high.
Lower alcohol in above-mentioned steps A is one or more the mixture in methanol, ethanol, propanol, isopropyl alcohol.
The solution of the 40%-70% of these lower alcohols, its polarity is suitable, can extract to greatest extent the Fructus Forsythiae ester glycoside in Fructus Forsythiae medical material.
Mass ratio between Fructus Forsythiae medical material and low-alcohol solution in above-mentioned steps A is 1:4-1:7.
Fructus Forsythiae medical material and low-alcohol solution adopt above ratio, can well extract the Fructus Forsythiae ester glycoside in Fructus Forsythiae medical material, have reduced again the consumption of low-alcohol solution and the time of concentrating under reduced pressure and energy consumption simultaneously.
Little polarity organic reagent in above-mentioned steps B is petroleum ether, cyclohexane extraction, hexane, pentane, chloroform or dichloromethane.
The extract of these little polarity organic reagents and ethyl acetate composition, can well extract the little polar impurity in diafiltration concentrated solution, thereby effectively improve purity and the content of the Fructus Forsythiae ester glycoside of prepared product.
In ethyl acetate/methanol mixed liquor in above-mentioned steps C, the volume ratio of ethyl acetate and methanol is 97:3-93:7.
Adopt the ethyl acetate/methanol mixed liquor of above ratio from the extracting mother liquid of back, to extract Fructus Forsythiae ester glycoside, make the yield of Fructus Forsythiae ester glycoside high, content is high.
Strong acid weak base salt soluble in water in above-mentioned steps C is CuSO
4, FeCl
2, (NH
4)
2sO
4, NH
4nO
3, NH
4cl, NH
4i, NH
4br, NH
4clO
4in one or more mixture.
The good water solubility of these strong acid weak base salts, the Ph value of mother solution can well be modulated to 3-5, thereby suppress dissociating of Fructus Forsythiae ester glycoside, and the polarity of mother solution is increased, Fructus Forsythiae ester glycoside can be dispensed in extract better in the time of extraction, to improve yield and the content of Fructus Forsythiae ester glycoside.
Below in conjunction with detailed description of the invention, the present invention is described in further detail.
Detailed description of the invention
Embodiment 1
A preparation method for Fructus Forsythiae total glycosides, comprises the steps:
A, diafiltration
By Fructus Forsythiae pulverizing medicinal materials to 20-40 order, be that the methanol solution that 4 times of Fructus Forsythiae quality of medicinal materials, volume fraction are 40% carries out the diafiltration of 36h to Fructus Forsythiae medical material by quality, percolate, percolate concentrating under reduced pressure at 60 DEG C of temperature obtains concentrated solution, the volume of concentrated solution is percolate 1/5;
This routine Fructus Forsythiae medical material is blue or green Fructus Forsythiae medical material, in the time of full maturity not, plucks the Fructus Forsythiae medical material obtaining.
B: extraction
Little polarity organic reagent-petroleum ether and ethyl acetate are mixed with to extract by the volume ratio of 1:1, then with the concentrated solution extraction of extract equity volume 3 times, discard extraction part mother solution;
C: saline extraction
Mother solution in step B adds (NH
4)
2sO
4, adjust mother solution pH to 5, then to use and the isopyknic ethyl acetate/methanol mixed liquor extraction of mother solution 6 times, combining extraction liquid, is evaporated to dryly, obtains Fructus Forsythiae total glycosides.Wherein, in ethyl acetate/methanol mixed liquor, the volume ratio of ethyl acetate and methanol is 97:3.
After tested, the Fructus Forsythiae total glycosides that this example makes, the mass content of its forsythiaside A is 51%.
Embodiment 2
A preparation method for Fructus Forsythiae total glycosides, comprises the steps:
A, diafiltration
By Fructus Forsythiae pulverizing medicinal materials to 20-40 order, be that the alcoholic solution that 7 times of Fructus Forsythiae quality of medicinal materials, volume fraction are 50% carries out the diafiltration of 42h to Fructus Forsythiae medical material by quality, percolate, percolate concentrating under reduced pressure at 55 DEG C of temperature obtains concentrated solution, the volume of concentrated solution is percolate 1/4;
This routine Fructus Forsythiae medical material is blue or green Fructus Forsythiae medical material.
B: extraction
Little polarity organic reagent-cyclohexane extraction and ethyl acetate are mixed with to extract by the volume ratio of 1:0.75, then with the concentrated solution extraction of extract equity volume 2 times, discard extraction part mother solution;
C: saline extraction
Mother solution in step B adds NH
4cl, adjusts mother solution pH to 4, then uses and the isopyknic ethyl acetate/methanol mixed liquor extraction of mother solution 5 times, and combining extraction liquid, is evaporated to dryly, obtains Fructus Forsythiae total glycosides.Wherein, in ethyl acetate/methanol mixed liquor, the volume ratio of ethyl acetate and methanol is 95:5.
After tested, the Fructus Forsythiae total glycosides that this example makes, the mass content of its forsythiaside A is 52%.
Embodiment 3
A preparation method for Fructus Forsythiae total glycosides, comprises the steps:
A, diafiltration
By Fructus Forsythiae pulverizing medicinal materials to 20-40 order, be that the alcoholic solution that 6 times of Fructus Forsythiae quality of medicinal materials, volume fraction are 70% carries out the diafiltration of 48h to Fructus Forsythiae medical material by quality, percolate, percolate concentrating under reduced pressure at 65 DEG C of temperature obtains concentrated solution, the volume of concentrated solution is percolate 1/4.5;
This routine Fructus Forsythiae medical material is blue or green Fructus Forsythiae medical material.
B: extraction
Little polarity organic reagent-hexane and ethyl acetate are mixed with to extract by the volume ratio of 1:0.5, then with the concentrated solution extraction of extract equity volume 4 times, discard extraction part mother solution;
C: saline extraction
Mother solution in step B adds NH
4nO
3, adjust mother solution pH to 3, then to use and the isopyknic ethyl acetate/methanol mixed liquor extraction of mother solution 4 times, combining extraction liquid, is evaporated to dryly, obtains Fructus Forsythiae total glycosides.Wherein, in ethyl acetate/methanol mixed liquor, the volume ratio of ethyl acetate and methanol is 93:7.
After tested, the Fructus Forsythiae total glycosides that this example makes, the mass content of its forsythiaside A is 50%.
Embodiment 4
A preparation method for Fructus Forsythiae total glycosides, comprises the steps:
A, diafiltration
By Fructus Forsythiae pulverizing medicinal materials to 20-40 order, be that the propanol solution that 7 times of Fructus Forsythiae quality of medicinal materials, volume fraction are 50% is carried out the diafiltration of 48h to Fructus Forsythiae medical material by quality, percolate, percolate concentrating under reduced pressure at 60 DEG C of temperature obtains concentrated solution, the volume of concentrated solution is percolate 1/4;
This routine Fructus Forsythiae medical material is blue or green Fructus Forsythiae medical material.
B: extraction
Little polarity organic reagent-pentane and ethyl acetate are mixed with to extract by the volume ratio of 1:1, then with the concentrated solution extraction of extract equity volume 2 times, discard extraction part mother solution;
C: saline extraction
Mother solution in step B adds CuSO
4, adjust mother solution pH to 4, then to use and the isopyknic ethyl acetate/methanol mixed liquor extraction of mother solution 5 times, combining extraction liquid, is evaporated to dryly, obtains Fructus Forsythiae total glycosides.Wherein, in ethyl acetate/methanol mixed liquor, the volume ratio of ethyl acetate and methanol is 95:5.
After tested, the Fructus Forsythiae total glycosides that this example makes, the mass content of its forsythiaside A is 53%.
Embodiment 5
A preparation method for Fructus Forsythiae total glycosides, comprises the steps:
A, diafiltration
By Fructus Forsythiae pulverizing medicinal materials to 20-40 order, be that the aqueous isopropanol that 5 times of Fructus Forsythiae quality of medicinal materials, volume fraction are 40% carries out the diafiltration of 42h to Fructus Forsythiae medical material by quality, percolate, percolate concentrating under reduced pressure at 55 DEG C of temperature obtains concentrated solution, the volume of concentrated solution is percolate 1/4;
This routine Fructus Forsythiae medical material is blue or green Fructus Forsythiae medical material.
B: extraction
Little polarity organic reagent-chloroform and ethyl acetate are mixed with to extract by the volume ratio of 1:0.75, then with the concentrated solution extraction of extract equity volume 3 times, discard extraction part mother solution;
C: saline extraction
Mother solution in step B adds NH
4i, adjusts mother solution pH to 4, then uses and the isopyknic ethyl acetate/methanol mixed liquor extraction of mother solution 5 times, and combining extraction liquid, is evaporated to dryly, obtains Fructus Forsythiae total glycosides.Wherein, in ethyl acetate/methanol mixed liquor, the volume ratio of ethyl acetate and methanol is 95:5.
After tested, the Fructus Forsythiae total glycosides that this example makes, the mass content of its forsythiaside A is 52%.
Embodiment 6
A preparation method for Fructus Forsythiae total glycosides, comprises the steps:
A, diafiltration
By Fructus Forsythiae pulverizing medicinal materials to 20-40 order, be that first, the alcohol mixed solution that 4 times of Fructus Forsythiae quality of medicinal materials, volume fraction are 60% carries out the diafiltration of 36h to Fructus Forsythiae medical material by quality, percolate, percolate concentrating under reduced pressure at 65 DEG C of temperature obtains concentrated solution, the volume of concentrated solution is percolate 1/5;
This routine Fructus Forsythiae medical material is blue or green Fructus Forsythiae medical material.
B: extraction
Little polarity organic reagent-dichloromethane and ethyl acetate are mixed with to extract by the volume ratio of 1:1, then with the concentrated solution extraction of extract equity volume 3 times, discard extraction part mother solution;
C: saline extraction
Mother solution in step B adds NH
4br, adjusts mother solution pH to 3, then uses and the isopyknic ethyl acetate/methanol mixed liquor extraction of mother solution 5 times, and combining extraction liquid, is evaporated to dryly, obtains Fructus Forsythiae total glycosides.Wherein, in ethyl acetate/methanol mixed liquor, the volume ratio of ethyl acetate and methanol is 95:5.
After tested, the Fructus Forsythiae total glycosides that this example makes, the mass content of its forsythiaside A is 52%.
Embodiment 7
A preparation method for Fructus Forsythiae total glycosides, comprises the steps:
A, diafiltration
By Fructus Forsythiae pulverizing medicinal materials to 20-40 order, be that the alcoholic solution that 4 times of Fructus Forsythiae quality of medicinal materials, volume fraction are 50% carries out the diafiltration of 42h to Fructus Forsythiae medical material by quality, percolate, percolate concentrating under reduced pressure at 55 DEG C of temperature obtains concentrated solution, the volume of concentrated solution is percolate 1/4;
This routine Fructus Forsythiae medical material is blue or green Fructus Forsythiae medical material.
B: extraction
Little polarity organic reagent-cyclohexane extraction and ethyl acetate are mixed with to extract by the volume ratio of 1:0.75, then with the concentrated solution extraction of extract equity volume 2 times, discard extraction part mother solution;
C: saline extraction
Mother solution in step B adds NH
4clO
4, adjust mother solution pH to 4, then to use and the isopyknic ethyl acetate/methanol mixed liquor extraction of mother solution 5 times, combining extraction liquid, is evaporated to dryly, obtains Fructus Forsythiae total glycosides.Wherein, in ethyl acetate/methanol mixed liquor, the volume ratio of ethyl acetate and methanol is 95:5.
After tested, the Fructus Forsythiae total glycosides that this example makes, the mass content of its forsythiaside A is 51%.
Embodiment 8
A preparation method for Fructus Forsythiae total glycosides, comprises the steps:
A, diafiltration
By Fructus Forsythiae pulverizing medicinal materials to 20-40 order, be that the methanol solution that 7 times of Fructus Forsythiae quality of medicinal materials, volume fraction are 50% carries out the diafiltration of 48h to Fructus Forsythiae medical material by quality, percolate, percolate concentrating under reduced pressure at 55 DEG C of temperature obtains concentrated solution, the volume of concentrated solution is percolate 1/5;
This routine Fructus Forsythiae medical material is blue or green Fructus Forsythiae medical material.
B: extraction
Little polarity organic reagent-cyclohexane extraction and ethyl acetate are mixed with to extract by the volume ratio of 1:0.75, then with the concentrated solution extraction of extract equity volume 4 times, discard extraction part mother solution;
C: saline extraction
Mother solution in step B adds FeCl
2, adjust mother solution pH to 4, then to use and the isopyknic ethyl acetate/methanol mixed liquor extraction of mother solution 5 times, combining extraction liquid, is evaporated to dryly, obtains Fructus Forsythiae total glycosides.Wherein, in ethyl acetate/methanol mixed liquor, the volume ratio of ethyl acetate and methanol is 93:7.
After tested, the Fructus Forsythiae total glycosides that this example makes, the mass content of its forsythiaside A is 51%.
Embodiment 9
A preparation method for Fructus Forsythiae total glycosides, comprises the steps:
A, diafiltration
By Fructus Forsythiae pulverizing medicinal materials to 20-40 order, be that the aqueous isopropanol that 6 times of Fructus Forsythiae quality of medicinal materials, volume fraction are 70% carries out the diafiltration of 36h to Fructus Forsythiae medical material by quality, percolate, percolate concentrating under reduced pressure at 60 DEG C of temperature obtains concentrated solution, the volume of concentrated solution is percolate 1/5;
This routine Fructus Forsythiae medical material is blue or green Fructus Forsythiae medical material.
B: extraction
Little polarity organic reagent-petroleum ether and ethyl acetate are mixed with to extract by the volume ratio of 1:0.5, then with the concentrated solution extraction of extract equity volume 2 times, discard extraction part mother solution;
C: saline extraction
Mother solution in step B adds NH
4cl and (NH
4)
2sO
4mixture, adjusts mother solution pH to 3, then uses and the isopyknic ethyl acetate/methanol mixed liquor extraction of mother solution 5 times, and combining extraction liquid, is evaporated to dryly, obtains Fructus Forsythiae total glycosides.Wherein, in ethyl acetate/methanol mixed liquor, the volume ratio of ethyl acetate and methanol is 95:5.
After tested, the Fructus Forsythiae total glycosides that this example makes, the mass content of its forsythiaside A is 52%.
Claims (7)
1. a preparation method for Fructus Forsythiae total glycosides, comprises the steps:
A: diafiltration
By Fructus Forsythiae pulverizing medicinal materials to 20-40 order, the low-alcohol solution that is 40%-70% by volume fraction carries out the diafiltration of 36-48h to Fructus Forsythiae medical material, percolate, percolate concentrating under reduced pressure at 55-65 DEG C of temperature obtains concentrated solution, the volume of concentrated solution is percolate 1/5～1/4;
B: extraction
Little polarity organic reagent and ethyl acetate are mixed with to extract by the volume ratio of 1:0.5～1, then with the concentrated solution extraction of extract equity volume 2-4 time, discard extraction part and obtain mother solution;
C: saline extraction
Mother solution in step B adds strong acid weak base salt soluble in water, adjusts mother solution pH to 3-5, then uses and the isopyknic ethyl acetate/methanol mixed liquor extraction of mother solution 4-6 time, and combining extraction liquid, is evaporated to dryly, obtains Fructus Forsythiae total glycosides.
2. require described method according to right 1, it is characterized in that, the Fructus Forsythiae medical material in described steps A is blue or green Fructus Forsythiae medical material.
3. require described method according to right 1, it is characterized in that, the lower alcohol in described steps A is one or more the mixture in methanol, ethanol, propanol, isopropyl alcohol.
4. require described method according to right 1, it is characterized in that, the mass ratio between Fructus Forsythiae medical material and low-alcohol solution in described steps A is 1:4-1:7.
5. require described method according to right 1, it is characterized in that, the little polarity organic reagent in described step B is petroleum ether, cyclohexane extraction, hexane, pentane, chloroform or dichloromethane.
6. require described method according to right 1, it is characterized in that, in the ethyl acetate/methanol mixed liquor in described step C, the volume ratio of ethyl acetate and methanol is 97:3-93:7.
7. require described method according to right 1, it is characterized in that, the strong acid weak base salt soluble in water in described step C is CuSO
4, FeCl
2, (NH
4)
2sO
4, NH
4nO
3, NH
4cl, NH
4i, NH
4br, NH
4clO
4in one or more mixture.
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| CN201410149410.2A CN103933127A (en) | 2014-04-14 | 2014-04-14 | Preparation method of forsythia total glycosides |
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ID=51181184
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Country Status (1)
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0616525A (en) * | 1991-07-19 | 1994-01-25 | Kanebo Ltd | Hair tonic cosmetic |
| CN101152261A (en) * | 2007-09-04 | 2008-04-02 | 北京理工大学 | Application of phenyl ethyl alcohol glycosides and xylogen glycosides component in forsythia (fruit or leaf) |
-
2014
- 2014-04-14 CN CN201410149410.2A patent/CN103933127A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0616525A (en) * | 1991-07-19 | 1994-01-25 | Kanebo Ltd | Hair tonic cosmetic |
| CN101152261A (en) * | 2007-09-04 | 2008-04-02 | 北京理工大学 | Application of phenyl ethyl alcohol glycosides and xylogen glycosides component in forsythia (fruit or leaf) |
Non-Patent Citations (3)
| Title |
|---|
| 叶良红等: "青翘和老翘中多种成分含量的比较", 《中药与临床》 * |
| 汪茂田等: "《天然有机化合物提取分离与结构鉴定》", 30 September 2004 * |
| 钟小群等: "不同提取工艺对连翘药材中连翘苷的影响", 《江西中医学院学报》 * |
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Application publication date: 20140723 |