CN106361798A - Extraction method of resin glycoside-type compound - Google Patents
Extraction method of resin glycoside-type compound Download PDFInfo
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- 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)
- A61K36/39—Convolvulaceae (Morning-glory family), e.g. bindweed
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention relates to an extraction method of a resin glycoside-type compound and belongs to the technical field of traditional Chinese medicines. The extraction method comprises carrying out chloroform-water heating backflow extraction on a medicinal sample, carrying out centrifugation precipitate removal orderly through methanol and chloroform, carrying out decoloring, carrying out silica gel column chromatography and gel chromatography purification, and carrying out drying. The invention provides the method for fast extraction of resin glycoside in convolvulaceous plants. The method has the advantages of simple operation, less solvent use amount, high purity and high yield and provides important reference for rapid purification of a resin glycoside-type compound.
Description
Technical field
The invention belongs to technical field of Chinese medicines, it is related to a kind of extracting method of Resin glycoside class compound.
Background technology
Resin glycoside is that Convolvulaceae is led a cow the main active of platymiscium, is a kind of middle medicinal substances being of great rarity, group
Become mainly by the macrolide having modified fatty acid, oligonucleotide chain and fatty acid to be formed, the sugar forming oligonucleotide chain mainly has d-
Glucose (d-glucose), l- rhamnose (l-rhamnose) and d- fucose (d-fucose) and d- quinovose (d-
quinovose)；Fatty acid includes modified fatty acid (replacing on the diverse location of glycosyl) and long-chain fatty acid (forms big ring
Lactone).Formed macrolide fatty acid mainly have four kinds, jalapinolic acid (jalapinic acid, that is, 11s- hydroxyl-
Hexadecanoic acid), convolvulinolic acid (convolvulinolic acid, i.e. 11s- hydroxyl-tetradecanoic acid), ipurolic acid
(the double hydroxyl-tetradecanoic acid of 3s, 11s-) and 3s, the double hydroxy-palmitic acid of 11s-.Resin glycoside is typically by a fatty acid conduct
Aglycon forms lactone with the monosaccharide of varying number, species, because the change of link position and multiple different substituents are esterified position
The change put, makes Resin glycoside class compound structure various.
Chinese patent cn102766180b discloses the method for purification of two active monomer compound and its product in Herba Saxifragae
The purposes of product, purification means are mainly Herba Saxifragae ethanol extraction, and extract uses petroleum ether, ethyl acetate extraction, second successively
Acetoacetic ester extract adopts the separation means such as silica gel column chromatography, medium pressure column chromatography, gel filtration chromatography again, separates from Herba Saxifragae
To two monomeric compounds (Quercetin 3-0- β-l- rhamnoside, Quercetin 5-o- beta -d-glucose- glycosides).This invented technology stream
Journey operating unit is many, and using the less eluant of polarity, purifying velocity is slower.
Disclose in International Journal of Triditional Chinese Medicine in November, 2012 volume 34 o. 11th to separate from cypress vine seed and set
Lipolysaccharide glycosides and a kind of first news flash of new tetrahydrofuran derivatives, the separation method mentioned in article is repeatedly related to column chromatography and divides
From, complex operation, the shortcomings of technological process is long.
At present, because Resin glycoside is more or less the same with the Organic substance dissolubility such as flavonoid, alkaloidss and Anthraquinones, existing
The purification of technology isolation technics thorough, technique is complex.Therefore, research and develop out the resin of a kind of purity and high income
The extracting method of glucoside compound is a difficult problem for current research.
Content of the invention
In order to solve the deficiencies in the prior art, the purpose of the present invention is to be to provide a kind of rapid extraction Resin glycoside class
The method of compound, can greatly save reagent and time, be to extract Resin glycoside from convolvulaceous plant to provide a kind of behaviour
Make the simple, universal method of low cost.
The invention provides a kind of extracting method of Resin glycoside class compound, comprise the following steps:
S1 slightly purifies: convolvulaceous plant remove impurity is dried, is crushed to 15-25 mesh, obtains coarse powder, added with chloroform-water mixed liquid
Circumfluence distillation, in described chloroform-water mixed liquid, chloroform percent by volume is 80-100%, filters, by extracting solution concentrating under reduced pressure,
Lyophilization obtains crude product a；
S2 removing impurity by means of precipitation: after crude product a addition methanol is completely dissolved, centrifugation, take supernatant concentrating under reduced pressure, cool drying,
Obtain fine powder, fine powder addition chloroform is completely dissolved, centrifugation, takes supernatant b；
S3 desolventing technology: supernatant b is carried out activated carbon decolorizing and processes 20-60 minute, filter, by filtrate reduced in volume,
Lyophilization obtains powder c；
S4 essence purification: powder c is carried out silica gel column chromatography, using chloroform-methanol mixed liquor or methylene chloride-methanol mixing
Liquid eluting, collects eluent, eluent concentrating under reduced pressure carries out gel chromatography again after lyophilization, using methanol-eluted fractions, collects
The eluent of the first and second column volumes, merges two post eluents, concentrating under reduced pressure, lyophilization, obtains final product.
Further, in described step s1, the consumption of chloroform-water mixed liquid and the solid-liquid ratio of coarse powder are 2-5ml:1g.
Further, heating and refluxing extraction 1-3 time in described step s1, each 1-3 hour.
Further, the methanol in described step s2 and crude product a liquid-solid ratio are 2-4ml:1g, chloroform and crude product a liquid-solid ratio
For 2-4ml:1g.
Further, the centrifugal condition in described step s2 is: 600-1000 rev/min, is centrifuged 5-15 minute.
Further, the granularity of activated carbon in described step s3 is 20-50 mesh.
Further, the silica gel column chromatography in described step s4 adopts dry column-packing, described sample silica gel and the powder c weight of mixing
Ratio for 1-3:1, fills post silica gel and powder c weight ratio for 30-100:1, described silica gel granularity is 100-300 mesh.
Further, in described chloroform-methanol mixed liquor, chloroform and the volume ratio of methanol are 30:1-5:1.
Further, in described methylene chloride-methanol mixed liquor, dichloromethane and the volume ratio of methanol are 30:1-5:1.
Convolvulaceous plant mainly includes flavone compound, alkaloid compound, anthraquinone analog compound and Resin glycoside
Class compound.Find, the extracting method of the Resin glycoside class compound being provided using the present invention can quickly be carried through exclusion test
Take the Resin glycoside class compound in convolvulaceous plant, and the extraction side of the Resin glycoside class compound being provided using the present invention
The yield of the Resin glycoside class compound that method is extracted is more than 2.65%, is a kind of carrying of ideal Resin glycoside class compound
Take method.
Compared with prior art, the extracting method of the Resin glycoside class compound that the present invention provides, can greatly save
Reagent and time, are to extract Resin glycoside from convolvulaceous plant to provide a kind of universal method simple to operate, low cost.
Specific embodiment
To further illustrate the present invention below by embodiment, but to be not limited to following examples.
Embodiment 1, a kind of extracting method of Resin glycoside class compound
S1 slightly purifies: Caulis et Folium Argyreia eacutae remove impurity is dried, is crushed to 20 mesh, obtains coarse powder, be heated to reflux carrying with chloroform-water mixed liquid
Take, the consumption of described chloroform-water mixed liquid and the solid-liquid ratio of coarse powder are 4ml:1g, chloroform volume in described chloroform-water mixed liquid
Percentage ratio is 90%, described heating and refluxing extraction 3 times, 2 hours every time, filters, by extracting solution concentrating under reduced pressure, lyophilization obtains
Crude product a；
S2 removing impurity by means of precipitation: after crude product a addition methanol is completely dissolved, described methanol and crude product a liquid-solid ratio are 3ml:1g,
It is centrifuged 10 minutes under conditions of 800 revs/min, take supernatant concentrating under reduced pressure, cool drying, obtain fine powder, fine powder is added chloroform
It is completely dissolved, described chloroform is 3ml:1g with crude product a liquid-solid ratio, be centrifuged 10 minutes under conditions of 800 revs/min, take supernatant
Liquid b；
S3 desolventing technology: supernatant b is carried out activated carbon decolorizing and processes 40 minutes, described granularity of activated carbon is 40 mesh, mistake
Filter, by filtrate reduced in volume, lyophilization obtains powder c；
S4 essence purification: powder c is carried out silica gel column chromatography, mixes sample silica gel and powder c weight ratio in described silica gel column chromatography
For 2:1, fill post silica gel and powder c weight ratio for 70:1, described silica gel granularity is 200 mesh, washes using chloroform-methanol mixed liquor
De-, collect eluent, in described chloroform-methanol mixed liquor, chloroform and the volume ratio of methanol are 25:1, by eluent concentrating under reduced pressure,
Carry out gel chromatography after lyophilization again, using methanol-eluted fractions, collect the eluent of the first and second column volumes, merge two posts and wash
De- liquid, concentrating under reduced pressure lyophilization, obtain final product.
Embodiment 2, a kind of extracting method of Resin glycoside class compound
S1 slightly purifies: Caulis et Folium Argyreia eacutae remove impurity is dried, is crushed to 15 mesh, obtains coarse powder, be heated to reflux carrying with chloroform-water mixed liquid
Take, the solid-liquid ratio of described chloroformic solution consumption and coarse powder is 2ml:1g, described heating and refluxing extraction 1 time, 3 hours every time, filter,
By extracting solution concentrating under reduced pressure, lyophilization obtains crude product a；
S2 removing impurity by means of precipitation: after crude product a addition methanol is completely dissolved, described methanol and crude product a liquid-solid ratio are 2ml:1g,
It is centrifuged 15 minutes under conditions of 600 revs/min, take supernatant concentrating under reduced pressure, cool drying, obtain fine powder, fine powder is added chloroform
It is completely dissolved, described chloroform is 4ml:1g with crude product a liquid-solid ratio, be centrifuged 5 minutes under conditions of 1000 revs/min, take supernatant
Liquid b；
S3 desolventing technology: supernatant b is carried out activated carbon decolorizing and processes 60 minutes, described granularity of activated carbon is 20 mesh, mistake
Filter, by filtrate reduced in volume, lyophilization obtains powder c；
S4 essence purification: powder c is carried out silica gel column chromatography, mixes sample silica gel and powder c weight ratio in described silica gel column chromatography
For 3:1, fill post silica gel and powder c weight ratio for 30:1, described silica gel granularity is 100 mesh, washes using chloroform-methanol mixed liquor
De-, collect eluent, in described chloroform-methanol mixed liquor, chloroform and the volume ratio of methanol are 30:1, by eluent concentrating under reduced pressure,
Carry out gel chromatography after lyophilization again, using methanol-eluted fractions, collect the eluent of the first and second column volumes, merge two posts and wash
De- liquid, concentrating under reduced pressure lyophilization, obtain final product.
Embodiment 3, a kind of extracting method of Resin glycoside class compound
S1 slightly purifies: Caulis et Folium Argyreia eacutae remove impurity is dried, is crushed to 25 mesh, obtains coarse powder, be heated to reflux carrying with chloroform-water mixed liquid
Take, the consumption of described chloroform-water mixed liquid and the solid-liquid ratio of coarse powder are 5ml:1g, chloroform volume in described chloroform-water mixed liquid
Percentage ratio is 80%, described heating and refluxing extraction 2 times, 1 hour every time, filters, by extracting solution concentrating under reduced pressure, lyophilization obtains
Crude product a；
S2 removing impurity by means of precipitation: after crude product a addition methanol is completely dissolved, methanol in described step s2 and crude product a solid-to-liquid ratio
For 4ml:1g, it is centrifuged 10 minutes under conditions of 1000 revs/min, takes supernatant concentrating under reduced pressure, cool drying, obtain fine powder, will
Fine powder adds chloroform to be completely dissolved, and described chloroform is 2ml:1g with crude product a solid-to-liquid ratio, is centrifuged 15 under conditions of 600 revs/min
Minute, take supernatant b；
S3 desolventing technology: supernatant b is carried out activated carbon decolorizing and processes 20 minutes, described granularity of activated carbon is 50 mesh, mistake
Filter, by filtrate reduced in volume, lyophilization obtains powder c；
S4 essence purification: powder c is carried out silica gel column chromatography, mixes sample silica gel and powder c weight ratio in described silica gel column chromatography
For 1:1, fill post silica gel and powder c weight ratio for 100:1, described silica gel granularity is 300 mesh, using methylene chloride-methanol mixing
Liquid eluting, collects eluent, and in described methylene chloride-methanol mixed liquor, dichloromethane and the volume ratio of methanol are 5:1, by eluting
Liquid concentrating under reduced pressure, carries out gel chromatography again after lyophilization, using methanol-eluted fractions, collect the eluting of the first and second column volumes
Liquid, merges two post eluents, concentrating under reduced pressure lyophilization, obtains final product.
Embodiment 4, a kind of extracting method of Resin glycoside class compound
S1 slightly purifies: Rhizoma Dioscoreae esculentae remove impurity is dried, is crushed to 20 mesh, obtains coarse powder, be heated to reflux carrying with chloroform-water mixed liquid
Take, the consumption of described chloroform-water mixed liquid and the solid-liquid ratio of coarse powder are 3ml:1g, described heating and refluxing extraction 3 times, 1 is little every time
When, filter, by extracting solution concentrating under reduced pressure, lyophilization obtains crude product a；
S2 removing impurity by means of precipitation: after crude product a addition methanol is completely dissolved, methanol in described step s2 and crude product a liquid-solid ratio
For 3ml:1g, it is centrifuged 10 minutes under conditions of 800 revs/min, takes supernatant concentrating under reduced pressure, cool drying, obtain fine powder, will be thin
Powder adds chloroform to be completely dissolved, and described chloroform is 4ml:1g with crude product a liquid-solid ratio, is centrifuged 10 under conditions of 1000 revs/min
Minute, take supernatant b；
S3 desolventing technology: supernatant b is carried out activated carbon decolorizing and processes 20 minutes, described granularity of activated carbon is 50 mesh, mistake
Filter, by filtrate reduced in volume, lyophilization obtains powder c；
S4 essence purification: powder c is carried out silica gel column chromatography, mixes sample silica gel and powder c weight ratio in described silica gel column chromatography
For 2:1, fill post silica gel and powder c weight ratio for 60:1, described silica gel granularity is 200 mesh, using methylene chloride-methanol mixed liquor
Eluting, collects eluent, and in described methylene chloride-methanol mixed liquor, dichloromethane and the volume ratio of methanol are 20:1, by eluting
Liquid concentrating under reduced pressure, carries out gel chromatography again after lyophilization, using methanol-eluted fractions, collect the eluting of the first and second column volumes
Liquid, merges two post eluents, concentrating under reduced pressure lyophilization, obtains final product.
Embodiment 5, a kind of extracting method of Resin glycoside class compound
S1 slightly purifies: cypress vine remove impurity is dried, is crushed to 20 mesh, obtains coarse powder, be heated to reflux carrying with chloroform-water mixed liquid
Take, the consumption of described chloroform-water mixed liquid and the solid-liquid ratio of coarse powder are 5ml:1g, described heating and refluxing extraction 3 times, 2 is little every time
When, filter, by extracting solution concentrating under reduced pressure, lyophilization obtains crude product a；
S2 removing impurity by means of precipitation: after crude product a addition methanol is completely dissolved, methanol in described step s2 and crude product a liquid-solid ratio
For 3ml:1g, it is centrifuged 10 minutes under conditions of 800 revs/min, takes supernatant concentrating under reduced pressure, cool drying, obtain fine powder, will be thin
Powder adds chloroform to be completely dissolved, and described chloroform is 2ml:1g with crude product a liquid-solid ratio, is centrifuged 10 points under conditions of 800 revs/min
Clock, takes supernatant b；
S3 desolventing technology: supernatant b is carried out activated carbon decolorizing and processes 20 minutes, described granularity of activated carbon is 50 mesh, mistake
Filter, by filtrate reduced in volume, lyophilization obtains powder c；
S4 essence purification: powder c is carried out silica gel column chromatography, mixes sample silica gel and powder c weight ratio in described silica gel column chromatography
For 2:1, fill post silica gel and powder c weight ratio for 70:1, described silica gel granularity is 200 mesh, using chloroform-methanol mixed liquor mixing
Liquid eluting, collects eluent, and in described chloroform-methanol mixed liquor, chloroform and the volume ratio of methanol are 15:1, and eluent is reduced pressure
Concentrate, after lyophilization, carry out gel chromatography again, using methanol-eluted fractions, collect the eluent of the first and second column volumes, merge
Two post eluents, concentrating under reduced pressure lyophilization, obtain final product.
Comparative example 1, a kind of extracting method of Resin glycoside class compound
Extracting method is different: the methanol heating and refluxing extraction being 90% with percent by volume in described step s1, remaining step
Suddenly similar to Example 1.
Comparative example 2, a kind of extracting method of Resin glycoside class compound
Extracting method is different: is extracted with the alcohol heating reflux that percent by volume is 90% in described step s1, remaining step
Suddenly similar to Example 1.
Comparative example 3, a kind of extracting method of Resin glycoside class compound
Extracting method is different: the consumption of described chloroform-water mixed liquid and the solid-liquid ratio of coarse powder are 8ml:1g, remaining step with
Embodiment 1 is similar to.
Test example one, the qualitative test of Resin glycoside class compound
1st, subjects: the product that the extraction of embodiment 1-5 obtains.
2nd, test method: the product obtaining is extracted to embodiment 1-5 and carries out flavone compound, alkaloid and Anthraquinones
The detection test of compound and sugar, polysaccharide and glycoside.
2.1st, reaction is known in flavone inspection: add a small amount of magnesium powder in the methanol solution of the product extracting gained in embodiment 1-5, and
Several concentrated hydrochloric acid of Deca.
2.2nd, reaction is known in alkaloid inspection: extracts in embodiment 1-5 and adds Dragendorff's reagent in the product of gained.
2.3rd, reaction is known in alkaloid inspection: adds Mayer's reagent in the product of embodiment 1-5 extraction gained.
2.4th, reaction is known in alkaloid inspection: extracts in embodiment 1-5 and adds Wagner's reagent in the product of gained.
2.5th, reaction is known in alkaloid inspection: extracts in embodiment 1-5 and adds tungstosilicic acid reagent in the product of gained.
2.6th, reaction is known in anthraquinone inspection: extracts in embodiment 1-5 and adds magnesium acetate methanol solution in the product of gained.
2.7th, reaction is known in sugar, polysaccharide and glycoside inspection: extracts in embodiment 1-5 and adds molish reagent in the product of gained.
3rd, result of the test:
3.1st, reaction: hydrochloric acid-magnesium powder reaction is known in flavone inspection, and rutin positive control solution hydrochloric acid-magnesium powder reaction assumes redness,
Negative controls redfree, the product obtaining in embodiment 1-5 carry out pyrite inspection know reaction also redfree produce it was demonstrated that product not
Containing flavone compound.
3.2nd, reaction: bismuth potassium iodide reaction is known in alkaloid inspection, and the reaction of berberine hydrochloride positive control solution bismuth potassium iodide occurs
Brown color precipitates, and negative controls no precipitate, and the product obtaining in embodiment 1-5 carries out bismuth potassium iodide reaction, and also no precipitation is produced
Life is not it was demonstrated that product contains alkaloid compound.
3.3rd, reaction: potassium mercuric iodide reaction is known in alkaloid inspection, and the reaction of berberine hydrochloride positive control solution potassium mercuric iodide occurs
Off-white color precipitates, and negative controls no precipitate, and the product obtaining in embodiment 1-5 carries out potassium mercuric iodide reaction, and also no precipitation is produced
Life is not it was demonstrated that product contains alkaloid compound.
3.4th, reaction: IKI reaction is known in alkaloid inspection, and berberine hydrochloride positive control solution IKI reflects
Existing tan precipitate, negative controls no precipitate, and the product obtaining in embodiment 1-5 carries out IKI reaction, and also no precipitation is produced
Life is not it was demonstrated that product contains alkaloid compound.
3.5th, reaction: tungstosilicic acid reaction is known in alkaloid inspection, and class in the reaction of berberine hydrochloride positive control solution bismuth potassium iodide
White precipitate, negative controls no precipitate, and the product obtaining in embodiment 1-5 carries out tungstosilicic acid reaction, and also no precipitation produces.Card
Bright product does not contain alkaloid compound.
3.6th, reaction: acetic acid reactive magnesium is known in anthraquinone inspection, and rheum emodin positive control solution acetic acid reactive magnesium assumes orange red, feminine gender
Comparison liquid is no orange red, and embodiment 1-5 product carries out the also no orange red generation of acetic acid reactive magnesium.Prove that product does not contain Anthraquinones
Compound.
3.7th, reaction: molish reaction is known in sugar, polysaccharide and glycoside inspection, and glucose positive control solution molish reaction occurs purple
Red ring, the no purplish red colour circle of negative controls, embodiment 1-5 product carries out molish reaction and aubergine ring.Prove product
In containing sugar, polysaccharide and glycoside class compound.
According to the qualitative analyses to product in embodiment 1-5, contain in the product of process purification that the present invention provides
Resin glycoside class compound, and do not contain the similar Organic substance flavone compound of other properties, alkaloid and Anthraquinones
Compound, illustrates that the product of present invention purification is Resin glycoside class compound, and purity is higher.
Test example two, the yield determination test of Resin glycoside class compound
1st, subjects: embodiment 1, embodiment 2, embodiment 3, comparative example 1, comparative example 2 and comparative example 3 extraction obtain
Resin glycoside class compound.
2nd, test method: take 20g Caulis et Folium Argyreia eacutae to adopt embodiment 1, embodiment 2, embodiment 3, comparative example 1, comparative example 2 and right
The extracting method of ratio 3 extracts the Resin glycoside class compound of Caulis et Folium Argyreia eacutae, weighs the material after extraction, calculates Resin glycoside class
The yield of compound.
3rd, result of the test:
Result of the test is as shown in table 1.
The yield determination test of table 1 Resin glycoside class compound
As shown in Table 1, the extracting method high income of the Resin glycoside class compound that the present invention provides, receives and reaches
2.65 ‰, above, the yield of embodiment 1 is 2.84 ‰, is most preferred embodiment.
Above-described embodiment only principle of the illustrative present invention and its effect, not for the restriction present invention.Any ripe
The personage knowing this technology all can carry out modifications and changes without prejudice under the spirit and the scope of the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
All equivalent modifications becoming or change, must be covered by the claim of the present invention.
Claims (9)
1. a kind of extracting method of Resin glycoside class compound is it is characterised in that comprise the following steps:
S1 slightly purifies: convolvulaceous plant remove impurity is dried, is crushed to 15-25 mesh, obtains coarse powder, heated back with chloroform-water mixed liquid
Stream extracts, and in described chloroform-water mixed liquid, the percent by volume of chloroform is 80-100%, filters, by extracting solution concentrating under reduced pressure, cold
Lyophilizing is dry, obtains crude product a；
S2 removing impurity by means of precipitation: after crude product a addition methanol is completely dissolved, centrifugation, take supernatant concentrating under reduced pressure, cool drying, obtain carefully
Powder, fine powder addition chloroform is completely dissolved, centrifugation, obtains supernatant b；
S3 desolventing technology: supernatant b is carried out activated carbon decolorizing and processes 20-60 minute, filter, filtrate reduced in volume freezes
It is dried, obtain powder c；
S4 essence purification: powder c is carried out silica gel column chromatography, is washed using chloroform-methanol mixed liquor or methylene chloride-methanol mixed liquor
De-, collect eluent, eluent concentrating under reduced pressure carries out gel chromatography again after lyophilization, using methanol-eluted fractions, collect first
With the eluent of the second column volume, merge two post eluents, concentrating under reduced pressure, lyophilization, obtain final product.
2. the extracting method of Resin glycoside class compound according to claim 1 is it is characterised in that chlorine in described step s1
Imitative-water mixed liquid is 2-5ml:1g with the solid-liquid ratio of coarse powder.
3. the extracting method of Resin glycoside class compound according to claim 1 is it is characterised in that add in described step s1
Circumfluence distillation 1-3 time, each 1-3 hour.
4. the extracting method of Resin glycoside class compound according to claim 1 is it is characterised in that in described step s2
Methanol is 2-4ml:1g with the liquid-solid ratio of crude product a, and chloroform is 2-4ml:1g with the liquid-solid ratio of crude product a.
5. the extracting method of Resin glycoside class compound according to claim 1 is it is characterised in that in described step s2
Centrifugal condition is: 600-1000 rev/min, is centrifuged 5-15 minute.
6. the extracting method of Resin glycoside class compound according to claim 1 is it is characterised in that in described step s3
Granularity of activated carbon is 20-50 mesh.
7. the extracting method of Resin glycoside class compound according to claim 1 is it is characterised in that in described step s4
Silica gel column chromatography adopts dry column-packing, and described sample silica gel and powder c weight ratio of mixing is for 1-3:1, described dress post silica gel and powder c weight
Amount ratio is 30-100:1, and described silica gel granularity is 100-300 mesh.
8. the extracting method of Resin glycoside class compound according to claim 1 is it is characterised in that described chloroform-methanol
In mixed liquor, chloroform and the volume ratio of methanol are 30:1-5:1.
9. the extracting method of Resin glycoside class compound according to claim 1 it is characterised in that described dichloromethane-
In methyl alcohol mixed liquor, dichloromethane and the volume ratio of methanol are 30:1-5:1.
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| CN108478619A (en) * | 2018-03-23 | 2018-09-04 | 南通大学 | Total Resin glycoside extract of field bindweed and preparation method thereof and medical usage |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108478619A (en) * | 2018-03-23 | 2018-09-04 | 南通大学 | Total Resin glycoside extract of field bindweed and preparation method thereof and medical usage |
| CN108478619B (en) * | 2018-03-23 | 2021-05-07 | 南通大学 | Convolvulus arvensis total resin glucoside extract, preparation method and medical application thereof |
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| CN106361798B (en) | 2019-04-26 |
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