CN110105411A - A kind of preparation method of silver forging glycosides - Google Patents
A kind of preparation method of silver forging glycosides Download PDFInfo
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- CN110105411A CN110105411A CN201910475452.8A CN201910475452A CN110105411A CN 110105411 A CN110105411 A CN 110105411A CN 201910475452 A CN201910475452 A CN 201910475452A CN 110105411 A CN110105411 A CN 110105411A
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- silver
- glycosides
- preparation
- forging glycosides
- extracting solution
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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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
Abstract
Glycosides technical field is forged the present invention relates to silver-colored, is related to a kind of preparation method of silver forging glycosides, comprising the following steps: S1, adds methanol after taking miracle fruit leaf to crush, is heated to reflux, extracts 3 times, filtering obtains silver linden glycoside extracting solution；S2, past silver linden glycoside extracting solution addition diatomite, stir, filtering, obtain destainer, concentration obtains medicinal extract later；S3, by medicinal extract it is water-dispersible after, adsorbed with adsorption resin column, then eluted with ethanol solution with 0.5-2.0BV/h, collect silver linden glycoside eluent；S4, silver linden glycoside solution is concentrated to get crystallization first product, adds the dissolving crystallized first product of ethanol water, filtered, recrystallized 2-3 times and obtain silver linden glycoside crystal finished product.This invention simplifies the conventional preparation techniques processes of silver forging glycosides preparation, overcome the defect that silver forging glycosides preparation process is complicated in the prior art and purity is not high, for the first time using low cost mysterious fruit tree leaves be prepared high-purity silver forging glycosides crystal, reach turn waste into wealth and high yield high-purity silver forging glycosides preparation purpose.
Description
Technical field
The present invention relates to silver to forge glycosides technical field, more specifically to a kind of preparation method of silver forging glycosides.
Background technique
Alpha-glucosidase restrainer be carbohydrate digestion final step inhibit disaccharide be degraded to monosaccharide, reach
It prevents and treats post prandial hyperglycemia and alleviates the purpose of hyperinsulinemia.Alpha-glucosidase restrainer is to I type and type II diabetes
It is applicable in, can also be combined with other oral hypoglycemic agents or insulin.Since they have the side effects such as abdominal distension, exhaust.Therefore, more
Start to favor in screening natural alpha-glucosidase restrainer from medicinal plant, to find new height come more scholars
The diabetes medicament of effect, low toxicity.
Silver forging glycosides (Tiliroside) is a kind of flavonoid glycoside compound, is yellow needles, mp.246~248 DEG C, molecule
Formula C30H26O13, molecular weight 594.52.Research shows that silver linden glycoside has good inhibiting effect to alpha-glucosidase.At present
Silver linden glycoside is mainly isolated from the plants such as oriental paperbush flower, Rose Mallow Root, Ipomoea batatas, Althaea roseal, Chinese bulbul aerial part.
Miracle fruit (Synsepalum dulcificum), also known as miracle fruit, dreamlike fruit or Synsepalum dulcuficum (Schum.) Daniell are Sapotaceae mind
Secret fruit category evergreen shrubs plant originates in West Africa area.Miracle fruit introduces Chinese Guangdong and Guangxi Provinces, Hainan, Yunnan the 1960s
It is planted with areas such as Fujian.Miracle fruit contains peculiar On Miraculin, it can change the sense of taste of people, makes to have originally sour
Food becomes sweet taste, thus is known as " the first under heaven surprise fruit ".Miracle fruit leaf is the leaf of mysterious fruit tree, and there has been no its changes at present
The research studied point and report.
It is rich in silver linden glycoside in previous research discovery miracle fruit according to us, content is up to 1.56%.So far, have no related
Extract the document report of isolated high content silver tiliacin from the plant of miracle fruit using simple production technology, and traditional silver
It is complicated to forge glycosides preparation process, preparation-obtained silver forging glycosides purity is not high.
Summary of the invention
In view of this, the present invention provides a kind of preparation method of silver forging glycosides, to solve silver forging glycosides preparation in the prior art
Complex process and the not high defect of purity.
A kind of preparation method of silver forging glycosides, comprising the following steps:
S1, it obtains silver forging glycosides extracting solution: adding methanol after taking miracle fruit leaf to crush, be heated to reflux 60-120 minutes, extract 3
Secondary, filtering obtains silver linden glycoside extracting solution；The solid-liquid ratio of mysterious fruit tree leaves and methanol in the step S1 is 1:8-1:15 (kg/
L)。
The decoloration of S2, silver forging glycosides extracting solution: being added diatomite toward silver linden glycoside extracting solution, stir, and filtering obtains destainer, dense
Medicinal extract is obtained after contracting；The additional amount of diatomite in the step S2 is total liquid measure 2%-6% of silver linden glycoside extracting solution.
S3, obtain silver forging glycosides eluent: by medicinal extract it is water-dispersible after, adsorbed with adsorption resin column, then with ethanol solution with
0.5-2.0BV/h elution, collects silver linden glycoside eluent；The percent by volume of ethanol solution in the step S3 is 30%-
60%.And the step S3 is collected silver linden glycoside eluent using TLC tracing detection.
S4, it obtains silver forging glycosides crystal: silver linden glycoside solution is concentrated to get crystallization first product, add ethanol water dissolving crystallized just
Product, filtering recrystallize 2-3 times and obtain silver linden glycoside crystal finished product.The purity of the obtained silver forging glycosides crystal of step S4 exists
95% or more.
It can be seen from the above technical scheme that the invention has the benefit that the present invention directly passes through smashing miracle fruit
Leaf is simultaneously added methanol and extracts to obtain silver forging glycosides extracting solution, then carries out decoloration separation to silver forging glycosides extracting solution again and is concentrated to give
Glycosides crystal is forged to silver, and the purity of silver forging glycosides crystal simplifies the conventional preparation techniques stream of silver forging glycosides preparation 95% or more
Journey overcomes the defect that silver forging glycosides preparation process is complicated in the prior art and purity is not high, utilizes the miracle fruit of low cost for the first time
Leaf be prepared high-purity silver forging glycosides crystal, reach turn waste into wealth and high yield high-purity silver forging glycosides preparation purpose.
Specific embodiment
Following example is for present invention be described in more detail, but embodiment does not do any type of limit to the present invention
Fixed, except illustrating, reagent that the present invention uses, method and apparatus are the conventional reagent of the art, method and apparatus,
But the invention is not limited in any way.
The embodiment of the invention discloses a kind of preparation methods of silver forging glycosides, comprising the following steps:
S1, it obtains silver forging glycosides extracting solution: adding methanol after taking miracle fruit leaf to crush, be heated to reflux 60-120 minutes, wherein
Solid-liquid ratio is 1:8-15 (kg/L), is extracted 3 times, and filtering obtains silver linden glycoside extracting solution；
The decoloration of S2, silver forging glycosides extracting solution: silver linden glycoside extracting solution is added to the diatomite of total liquid measure 2%-6%, is stirred, mistake
Filter obtains destainer, obtains medicinal extract after concentration；
S3, obtain silver forging glycosides eluent: by medicinal extract it is water-dispersible after, adsorbed with large pore resin absorption column, then with volume hundred
Divide than being that the ethanol solution of 30%-60% is eluted with 0.5-2.0BV/h, using TLC tracing detection, collects silver linden glycoside eluent；
S4, it obtains silver forging glycosides crystal: silver linden glycoside solution being concentrated into small size, crystallization is placed, ethanol water is added to dissolve,
Filtering recrystallizes 2-3 times and obtains the silver linden glycoside crystal of 95% or more purity.
More specifically, the invention also discloses a kind of specific preparation flows of the preparation method of silver forging glycosides:
Embodiment 1:
S1, it obtains silver forging glycosides extracting solution: after taking miracle fruit leaf to crush plus methanol, being heated to reflux 120 minutes, wherein feed liquid
Than extracting 3 times for 1:8 (kg/L), filtering obtains silver linden glycoside extracting solution；
Silver linden glycoside extracting solution: being added the diatomite of total liquid measure 2%, stirred by the decoloration of S2, silver forging glycosides extracting solution, filtering,
Destainer is obtained, obtains medicinal extract after concentration；
S3, obtain silver forging glycosides eluent: by medicinal extract it is water-dispersible after, adsorbed with large pore resin absorption column, then with volume hundred
Divide than being eluted for 30% ethanol solution with 2.0BV/h, using TLC tracing detection, collects silver linden glycoside eluent；
S4, it obtains silver forging glycosides crystal: silver linden glycoside solution being concentrated into small size, crystallization is placed, ethanol water is added to dissolve,
Filtering recrystallizes 3 obtained silver linden glycoside crystal, remembers sample 1.
Embodiment 2:
S1, it obtains silver forging glycosides extracting solution: after taking miracle fruit leaf to crush plus methanol, being heated to reflux 120 minutes, wherein feed liquid
Than extracting 3 times for 1:15 (kg/L), filtering obtains silver linden glycoside extracting solution；
Silver linden glycoside extracting solution: being added the diatomite of total liquid measure 2%, stirred by the decoloration of S2, silver forging glycosides extracting solution, filtering,
Destainer is obtained, obtains medicinal extract after concentration；
S3, obtain silver forging glycosides eluent: by medicinal extract it is water-dispersible after, adsorbed with large pore resin absorption column, then with volume hundred
Divide than being eluted for 30% ethanol solution with 2.0BV/h, using TLC tracing detection, collects silver linden glycoside eluent；
S4, it obtains silver forging glycosides crystal: silver linden glycoside solution being concentrated into small size, crystallization is placed, ethanol water is added to dissolve,
Filtering recrystallizes 3 obtained silver linden glycoside crystal, is denoted as sample 2.
Embodiment 3:
S1, it obtains silver forging glycosides extracting solution: after taking miracle fruit leaf to crush plus methanol, being heated to reflux 120 minutes, wherein feed liquid
Than extracting 3 times for 1:13 (kg/L), filtering obtains silver linden glycoside extracting solution, and being heated to reflux temperature is 100 degrees Celsius；
Silver linden glycoside extracting solution: being added the diatomite of total liquid measure 5%, stirred by the decoloration of S2, silver forging glycosides extracting solution, filtering,
Destainer is obtained, obtains medicinal extract after concentration；
S3, obtain silver forging glycosides eluent: by medicinal extract it is water-dispersible after, adsorbed with large pore resin absorption column, then with volume hundred
Divide than being eluted for 30% ethanol solution with 2.0BV/h, using TLC tracing detection, collects silver linden glycoside eluent；
S4, it obtains silver forging glycosides crystal: silver linden glycoside solution being concentrated into small size, crystallization is placed, ethanol water is added to dissolve,
Filtering recrystallizes 3 obtained silver linden glycoside crystal, is denoted as sample 3.
Embodiment 4:
S1, it obtains silver forging glycosides extracting solution: after taking miracle fruit leaf to crush plus methanol, being heated to reflux 120 minutes, wherein feed liquid
Than extracting 3 times for 1:13 (kg/L), filtering obtains silver linden glycoside extracting solution；
Silver linden glycoside extracting solution: being added the diatomite of total liquid measure 5%, stirred by the decoloration of S2, silver forging glycosides extracting solution, filtering,
Destainer is obtained, obtains medicinal extract after concentration；
S3, obtain silver forging glycosides eluent: by medicinal extract it is water-dispersible after, adsorbed with large pore resin absorption column, then with volume hundred
Divide than being eluted for 50% ethanol solution with 2.0BV/h, using TLC tracing detection, collects silver linden glycoside eluent；
S4, it obtains silver forging glycosides crystal: silver linden glycoside solution being concentrated into small size, crystallization is placed, ethanol water is added to dissolve,
Filtering recrystallizes 3 obtained silver linden glycoside crystal, remembers sample 4.
Comparative example 5
S1, it obtains silver forging glycosides extracting solution: after taking miracle fruit leaf to crush plus methanol, being heated to reflux 120 minutes, wherein feed liquid
Than extracting 3 times for 1:5 (kg/L), filtering obtains silver linden glycoside extracting solution；
Silver linden glycoside extracting solution: being added the diatomite of total liquid measure 2%, stirred by the decoloration of S2, silver forging glycosides extracting solution, filtering,
Destainer is obtained, obtains medicinal extract after concentration；
S3, obtain silver forging glycosides eluent: by medicinal extract it is water-dispersible after, adsorbed with large pore resin absorption column, then with volume hundred
Divide than being eluted for 30% ethanol solution with 2.0BV/h, using TLC tracing detection, collects silver linden glycoside eluent；
S4, it obtains silver forging glycosides crystal: silver linden glycoside solution being concentrated into small size, crystallization is placed, ethanol water is added to dissolve,
Filtering recrystallizes 3 obtained silver linden glycoside crystal, remembers contrast sample 5.
Comparative example 6
S1, it obtains silver forging glycosides extracting solution: after taking miracle fruit leaf to crush plus methanol, being heated to reflux 120 minutes, wherein feed liquid
Than extracting 3 times for 1:16 (kg/L), filtering obtains silver linden glycoside extracting solution；
Silver linden glycoside extracting solution: being added the diatomite of total liquid measure 2%, stirred by the decoloration of S2, silver forging glycosides extracting solution, filtering,
Destainer is obtained, obtains medicinal extract after concentration；
S3, obtain silver forging glycosides eluent: by medicinal extract it is water-dispersible after, adsorbed with large pore resin absorption column, then with volume hundred
Divide than being eluted for 30% ethanol solution with 2.0BV/h, using TLC tracing detection, collects silver linden glycoside eluent；
S4, it obtains silver forging glycosides crystal: silver linden glycoside solution being concentrated into small size, crystallization is placed, ethanol water is added to dissolve,
Filtering recrystallizes 3 obtained silver linden glycoside crystal, remembers contrast sample 6.
Silver linden glycoside crystal concentration is carried out to the obtained sample of above-described embodiment to measure to obtain table 1:
1 silver linden glycoside crystal concentration of table measures table (detecting using HPLC)
As can be seen from Table 1, the concentration highest of silver linden glycoside crystal prepared by embodiment 4, and it is made using the technical program
Standby tiliacin crystal can be prepared into function, and concentration is all larger than 95%.Obviously, the present invention directly passes through the mysterious fruit tree leaves of smashing simultaneously
Methanol is added to extract to obtain silver forging glycosides extracting solution, decoloration separation then is carried out to silver forging glycosides extracting solution again and is concentrated to get silver-colored forging
Glycosides crystal, and the purity of silver forging glycosides crystal simplifies the conventional preparation techniques process of silver forging glycosides preparation, overcomes 95% or more
The defect that silver forging glycosides preparation process is complicated in the prior art and purity is not high is prepared using the mysterious fruit tree leaves of low cost for the first time
Obtain high-purity silver forging glycosides crystal, reach turn waste into wealth and high yield high-purity silver forging glycosides preparation purpose.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment cross-reference.
The foregoing description of the disclosed embodiments makes professional and technical personnel in the field can be realized the present invention.To these
A variety of modifications of embodiment will be readily apparent to those skilled in the art, general original as defined herein
Reason can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention will not
Be intended to be limited to the embodiments shown herein, and be to fit to it is consistent with the principles and novel features disclosed in this article most
Wide range.
Claims (6)
1. a kind of preparation method of silver forging glycosides, which comprises the following steps:
S1, it obtains silver forging glycosides extracting solution: adding methanol after taking miracle fruit leaf to crush, be heated to reflux 60-120 minutes, extract 3 times,
Filtering, obtains silver linden glycoside extracting solution；
The decoloration of S2, silver forging glycosides extracting solution: being added diatomite toward silver linden glycoside extracting solution, stir, and filtering obtains destainer, it is concentrated
Medicinal extract is obtained afterwards；
S3, obtain silver forging glycosides eluent: by medicinal extract it is water-dispersible after, adsorbed with adsorption resin column, then with ethanol solution with 0.5-
2.0BV/h elution, collects silver linden glycoside eluent；
S4, it obtains silver forging glycosides crystal: silver linden glycoside solution being concentrated to get crystallization first product, adds the dissolving crystallized first product of ethanol water,
Filtering recrystallizes 2-3 times and obtains silver linden glycoside crystal finished product.
2. a kind of preparation method of silver forging glycosides according to claim 1, which is characterized in that the miracle fruit in the step S1
The solid-liquid ratio of leaf and methanol is 1:8-1:15 (kg/L).
3. a kind of preparation method of silver forging glycosides according to claim 1, which is characterized in that the diatomite in the step S2
Additional amount be silver linden glycoside extracting solution total liquid measure 2%-6%.
4. a kind of preparation method of silver forging glycosides according to claim 1, which is characterized in that the ethyl alcohol in the step S3 is molten
The percent by volume of liquid is 30%-60%.
5. it is according to claim 1 it is a kind of silver forging glycosides preparation method, which is characterized in that the step S3 using
TLC tracing detection is collected silver linden glycoside eluent.
6. a kind of preparation method of silver forging glycosides according to claim 1, which is characterized in that the obtained silver of step S4
The purity of glycosides crystal is forged 95% or more.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304161A (en) * | 2011-07-06 | 2012-01-04 | 南京泽朗医药科技有限公司 | Method for extracting and purifying tiliroside |
| CN105001286A (en) * | 2015-07-23 | 2015-10-28 | 昆明理工大学 | Method for extracting tiliroside from Tibetan drug scindapsus aureus |
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2019
- 2019-06-03 CN CN201910475452.8A patent/CN110105411B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304161A (en) * | 2011-07-06 | 2012-01-04 | 南京泽朗医药科技有限公司 | Method for extracting and purifying tiliroside |
| CN105001286A (en) * | 2015-07-23 | 2015-10-28 | 昆明理工大学 | Method for extracting tiliroside from Tibetan drug scindapsus aureus |
Non-Patent Citations (2)
| Title |
|---|
| RENATA NOWAK: "Separation and Quantification of Tiliroside from Plant Extracts by SPE/RP-HPLC", 《PHARMACEUTICAL BIOLOGY》 * |
| 陈琪等: "神秘果化学成分和生物活性研究进展", 《中国中医药现代远程教育》 * |
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