CN102746362A - Method for extracting refined astragaloside from astragaliradix - Google Patents
Method for extracting refined astragaloside from astragaliradix Download PDFInfo
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Abstract
The invention discloses a method for extracting refined astragaloside from astragaliradix. Astragaloside is a lanolin alcohol-form tetracyclic triterpenoid saponin compound. A Chinese herbal medicine astragaliradix is rich in astragaloside. The method utilizes a series of high-efficiency extraction, separation and purification technical processes of ethanol reflux extraction, alkaline hydrolysis, macroporous resin purification, ion-exchange resin decoloration and recrystallization to realize extraction of a target compound which is white powder and has a yield more than 0.07% and purity more than 99%. The method is simple, can be operated easily, does not produce pollution and is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of method of from safflower, extracting refining astragalus first glycosides.
Background technology
The Radix Astragali is the dry root of leguminous plants Radix Astagali Astragalus membranaceus (Fisch.) Bge. var. mongholicus (Bge.) Hsiao or Radix Astragali Astragalus membranaceus (Fisch.) Bge..Radix Astragali is a mesophyte, is born under mountain region border, shrubbery and the sparse woods.Be distributed in Yanshan mountain range, Mount Taishan, Xiaowutai Shan Mountain, Hengshan Mountain, Wutai Mountain, loess plateau, Tai Yueshan, the Qinling Mountains, the north of Hengduan mountain range in large and small Xing'an Mountains, Wanda Mountain, Zhang Guangcai mountain range, master mountain range, Changbai Mountain and mountain region, east, Liaoning and North China in Altai Mountains, the northeast of Xinjiang of China; Radix Astagali is non-irrigated mesophyte, is born in ground such as upland meadow, shrubbery, border, limes marginis.Siklingelei white tone tin that is distributed in the Inner Mongol is reined in, Huang gang, Keshiketeng Banner beam and a white tone pile of stones, and the mountain region, the Yanshan Mountain of North China, Daqunshan Mountains, rough sweat mountain, Xiaowutai Shan Mountain, Hengshan Mountain, Wutai Mountain, mountain, Lvliang City are northern.The Radix Astragali has effects such as invigorating QI to consolidate the body surface resistance, diuresis holder poison, apocenosis, expelling pus and promoting granulation.Show through modern study: the pharmacologically active of the Radix Astragali is varied; It has many-sided effect to cardiovascular systems; Also have antitumor and enhance immunity function, lowering blood glucose, hypotensive, endocrine regulation function simultaneously; And its prevention and health care function more and more receives people's attention, thereby uses very extensively.The chemical ingredients of the Radix Astragali is more, mainly contains saponins, flavonoid and polysaccharide etc., and wherein saponins compound has Radix Astragali saponin and soybean saponin thereof, and flavonoid compound has flavones, NOVASOY 400, isoflavan and red sandalwood alkane four big classes.Still contain compositions such as monose, amino acid, protein, coffic acid, chlorogenicacid, palmitinic acid, β-Gu Zaichun, daucosterol in addition.Show that after deliberation saponins compound is one of important composition of Radix Astragali effective substance, Cyclosiversioside F (astragatoside IV) then is one of main active ingredient of the Radix Astragali.
Cyclosiversioside F is a kind of tetracyclic triterpene saponin(e of isocholesterol shape, and molecular formula is C
14H
68O
14, relative molecular mass is 784, modern pharmacology show Cyclosiversioside F have cardiovascular, the cardiac stimulant of protection, neuroprotective system and endothelial barrier function damage, anti-gastric-ulcer, anti-ageing, protect effects such as liver, antalgic and sedative, diuresis and promotion secretion of insulin.Cyclosiversioside F is the important index property composition of estimating Milkvetch Root at present and containing the Milkvetch Root preparation, and the content of Cyclosiversioside F in Milkvetch Root is very low, is about 0.04%, though more stable, extraction separation is very difficult.Along with the continuation of research deeply, about the new installation and the novel method of the extraction separation of Cyclosiversioside F will constantly be emerged in large numbers.
One Chinese patent application numbers 200310108915.6 discloses a kind of method that from Chinese medicine astragalus, prepares Cyclosiversioside F, with astragalus root pulverizing, water refluxing extraction, macroporous resin removal of impurities, decolouring, centrifugal.But the rate of transform of this method Cyclosiversioside F and purity are not high.One Chinese patent application numbers 200710043678.8 discloses a kind of Cyclosiversioside F preparation method, is to be raw material with the Chinese medicine astragalus, comprises steps such as water extraction, alkaline purification, macroporous resin removal of impurities, crystallization.This method Cyclosiversioside F recovery is low, and gained Cyclosiversioside F purity is not high.One Chinese patent application numbers 200410014786.9 discloses a kind of preparation method of Cyclosiversioside F and the new purposes in pharmacy thereof.Be with alcohol reflux, alkaline hydrolysis, organic solvent extraction, recrystallizing methanol etc. with Milkvetch Root.But this method has been used organic solvent, and the rate of transform of Cyclosiversioside F and purity are not high yet.One Chinese patent application numbers 200910250347.0 discloses a kind of extraction process of Cyclosiversioside F.With raw material section or meal enzymolysis, water carry, extract, refining.But organic solvent is used in this invention, and the yield of Cyclosiversioside F and purity are not high.One Chinese patent application numbers 201010101933.1 discloses the method for a kind of extraction from Chinese medicine astragalus, separation and purifying Astragaloside IV, adopts enzymolysis, basic hydrolysis, extraction, macroporous resin enrichment and silica gel column chromatography etc.This step application organic solvent, and the yield of Cyclosiversioside F is not high.One Chinese patent application numbers 200910234071.7 discloses a kind of method that from the Radix Astragali, prepares Cyclosiversioside F.With the Radix Astragali is raw material, liming hydrolysis, ultrafiltration removal of impurities, macroporous resin removal of impurities, recrystallization.The yield of this method Cyclosiversioside F and purity are not high.One Chinese patent application numbers 200510020977.0 discloses a kind of preparation method of purity astragaloside.This method is a raw material with the Chinese medicine astragalus, extracts, enrichment, removal of impurities, hydrolysis, extraction and refining etc.This method has been used organic solvent, is unfavorable for big production.One Chinese patent application numbers 200610012687.6 discloses a kind of extraction preparation method of Cyclosiversioside F.This step is that water is carried, alcohol precipitation, basic hydrolysis, decolouring etc.The purity of this method Cyclosiversioside F is not high.One Chinese patent application numbers 200910078504.4 discloses a kind of preparation method of Cyclosiversioside F.This method is extracted, macroporous resin column is separated, soda acid removal of impurities, basic hydrolysis, recrystallization etc.It is darker that this method has been used the color of organic solvent and Cyclosiversioside F elaboration.One Chinese patent application numbers 200410007963.0 discloses a kind of preparation method and bulk drug and preparation of Cyclosiversioside F bulk drug.This method adopts extraction, alkaline purification, extraction, step such as refining.Yield and purity that organic solvent and Cyclosiversioside F have been used in this invention are not high.One Chinese patent application numbers 200910060581.7 discloses a kind of working method for preparing Cyclosiversioside F.Steps such as this method adopts and extract, centrifugal, ultrafiltration.But the yield of this method Cyclosiversioside F and purity are not high.One Chinese patent application numbers 200910232203.2 discloses a kind of preparation method who treats the high-purity astragaloside of diabetic complication ephrosis, peripheral neuropathy.Through steps such as extraction using alcohol, basic hydrolysis, removal of impurities, silica gel purification, recrystallizations.But this method has been used organic solvent, is not suitable for big production, and the yield of Cyclosiversioside F is not high.
Summary of the invention
The present invention provides a kind of method of from the Radix Astragali, extracting refining astragalus first glycosides, and this method comprises the steps:
A, extraction: take by weighing Radix Astragali medicine materical crude slice, add 6-12 at every turn and doubly measure the 60%-80% ethanolic soln, heating and refluxing extraction 2-3 time, each 1h-3h soaks 20min-40min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, and be settled to soup: the medicinal material envelope-bulk to weight ratio is 1:1-2:1, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, and the NaOH solution according to the ratio adding 1mol/L that adds 0.005g-0.02gNaOH in the 1g medicinal material is heated to 60 ℃-100 ℃; Stir; Continuous backflow 2h-6h to 0.04-0.4g medicinal material/ml, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: according to the medicinal material amount: the amount of resin weight ratio is that 2:1-1:2 takes by weighing macroporous adsorbent resin, and the blade diameter length ratio of packing into is the chromatography column of 1:3-1:12, with 95% ethanol and zero(ppm) water processing totally; With on the alkaline hydrolyzate appearance, absorption flow velocity be 6 times of column volumes/hour, saturated 1h-3h; Carry out wash-out with the zero(ppm) water of 10 times of-20 times of column volumes and remove sugar, elution flow rate be 12 times of column volumes/hour; With the NaOH solution removal of impurities of 10 times of-20 times of column volume 0.1mol/L, elution flow rate be 12 times of column volumes/hour, dash to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 7 times of column volumes 40%, elution flow rate be 12 times of column volumes/hour; Ethanolic soln with 10 times of-20 times of column volumes 60% carries out wash-out, elution flow rate be 12 times of column volumes/hour, collect 60% ethanol eluate, refined solution A;
D, purifying for the second time: according to the medicinal material amount: the amount of resin weight ratio is that 3.2:1-1:1 takes by weighing weakly basic anion exchange resin; The blade diameter length ratio of packing into is the chromatography column of 1:3-1:10; Use the acid-alkali treatment weakly basic anion exchange resin, finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, flow velocity be 3.6 times of column volumes/hour, collect effluent; Flow through the weak anion resin post with 3 times of-5 times of column volume 60% ethanolic solns, collect effluent; Two-part effluent merging is concentrated into 6.4g medicinal material/ml-16g medicinal material/ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
The present invention extracts refining astragalus first glycosides from the Radix Astragali method is preferably and comprises the steps:
A, extraction: take by weighing Radix Astragali medicine materical crude slice, add 12 times of amount 80% ethanolic solns at every turn, heating and refluxing extraction 2 times, each 3h soaks 20min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, and be settled to soup: the medicinal material envelope-bulk to weight ratio is 2:1, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, and the NaOH solution according to the ratio adding 1mol/L that adds 0.005gNaOH in the 1g medicinal material is heated to 60 ℃, stirs, and continuous backflow 6h to 0.4g medicinal material/ml, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: according to the medicinal material amount: the amount of resin weight ratio is that 2:1 takes by weighing macroporous adsorbent resin, and the blade diameter length ratio of packing into is the chromatography column of 1:3, with 95% ethanol and zero(ppm) water processing totally; With on the alkaline hydrolyzate appearance, absorption flow velocity be 6 times of column volumes/hour, saturated 3h; Carry out wash-out with the zero(ppm) water of 20 times of column volumes and remove sugar, elution flow rate be 12 times of column volumes/hour; With the NaOH solution removal of impurities of 10 times of column volume 0.1mol/L, elution flow rate be 12 times of column volumes/hour, dash to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 7 times of column volumes 40%, elution flow rate be 12 times of column volumes/hour; Ethanolic soln with 10 times of column volumes 60% carries out wash-out, elution flow rate be 12 times of column volumes/hour, collect 60% ethanol eluate, refined solution A;
D, purifying for the second time: according to the medicinal material amount: the amount of resin weight ratio is that 3.2:1 takes by weighing weakly basic anion exchange resin, and the blade diameter length ratio of packing into is the chromatography column of 1:10, uses the acid-alkali treatment weakly basic anion exchange resin, and finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, flow velocity be 3.6 times of column volumes/hour, collect effluent; Flow through the weak anion resin post with 5 times of column volume 60% ethanolic solns, collect effluent; Two-part effluent merging is concentrated into 16g medicinal material/ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
The present invention extracts refining astragalus first glycosides from the Radix Astragali method also is preferably and comprises the steps:
A, extraction: take by weighing Radix Astragali medicine materical crude slice, add 6 times of amount 60% ethanolic solns at every turn, heating and refluxing extraction 3 times, each 1h soaks 40min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, and be settled to soup: the medicinal material envelope-bulk to weight ratio is 1:1, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, and the NaOH solution according to the ratio adding 1mol/L that adds 0.02gNaOH in the 1g medicinal material is heated to 100 ℃, stirs, and continuous backflow 2h to 0.04g medicinal material/ml, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: according to the medicinal material amount: the amount of resin weight ratio is that 1:2 takes by weighing macroporous adsorbent resin, and the blade diameter length ratio of packing into is the chromatography column of 1:12, with 95% ethanol and zero(ppm) water processing totally; With on the alkaline hydrolyzate appearance, absorption flow velocity be 6 times of column volumes/hour, saturated 1h; Carry out wash-out with the zero(ppm) water of 10 times of column volumes and remove sugar, elution flow rate be 12 times of column volumes/hour; With the NaOH solution removal of impurities of 20 times of column volume 0.1mol/L, elution flow rate be 12 times of column volumes/hour, dash to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 7 times of column volumes 40%, elution flow rate be 12 times of column volumes/hour; Ethanolic soln with 20 times of column volumes 60% carries out wash-out, elution flow rate be 12 times of column volumes/hour, collect 60% ethanol eluate, refined solution A;
D, purifying for the second time: according to the medicinal material amount: the amount of resin weight ratio is that 1:1 takes by weighing weakly basic anion exchange resin, and the blade diameter length ratio of packing into is the chromatography column of 1:3, uses the acid-alkali treatment weakly basic anion exchange resin, and finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, flow velocity be 3.6 times of column volumes/hour, collect effluent; Flow through the weak anion resin post with 3 times of column volume 60% ethanolic solns, collect effluent; Two-part effluent merging is concentrated into 6.4g medicinal material/ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
The present invention extracts refining astragalus first glycosides from the Radix Astragali method also is preferably and comprises the steps:
A, extraction: take by weighing Radix Astragali medicine materical crude slice, add 9 times of amount 70% ethanolic solns at every turn, heating and refluxing extraction 3 times, each 2h soaks 30min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, and be settled to soup: the medicinal material envelope-bulk to weight ratio is 1.5:1, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, and the NaOH solution according to the ratio adding 1mol/L that adds 0.015gNaOH in the 1g medicinal material is heated to 80 ℃, stirs, and continuous backflow 4h to 0.24g medicinal material/ml, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: according to the medicinal material amount: the amount of resin weight ratio is that 1:1 takes by weighing macroporous adsorbent resin, and the blade diameter length ratio of packing into is the chromatography column of 2:15, with 95% ethanol and zero(ppm) water processing totally; With on the alkaline hydrolyzate appearance, absorption flow velocity be 6 times of column volumes/hour, saturated 2h; Carry out wash-out with the zero(ppm) water of 15 times of column volumes and remove sugar, elution flow rate be 12 times of column volumes/hour; With the NaOH solution removal of impurities of 15 times of column volume 0.1mol/L, elution flow rate be 12 times of column volumes/hour, dash to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 7 times of column volumes 40%, elution flow rate be 12 times of column volumes/hour; Ethanolic soln with 15 times of column volumes 60% carries out wash-out, elution flow rate be 12 times of column volumes/hour, collect 60% ethanol eluate, refined solution A;
D, purifying for the second time: according to the medicinal material amount: the amount of resin weight ratio is that 2.1:1 takes by weighing weakly basic anion exchange resin, and the blade diameter length ratio of packing into is the chromatography column of 2:13, uses the acid-alkali treatment weakly basic anion exchange resin, and finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, flow velocity be 3.6 times of column volumes/hour, collect effluent; Flow through the weak anion resin post with 4 times of column volume 60% ethanolic solns, collect effluent; Two-part effluent merging is concentrated into 11.2g medicinal material/ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
The present invention extracts employed macroporous adsorbent resin in the method for refining astragalus first glycosides and is preferably a kind of in HPD722, HPD100, HPD910, AB-8, the D101 resin from the Radix Astragali, the weak-base ion-exchange resin that uses is preferably 330 resins.
The present invention extracts refining astragalus first glycosides from the Radix Astragali method further is preferably and comprises the steps:
A, extraction: take by weighing Radix Astragali medicine materical crude slice, add 8 times of amount 80% ethanolic solns at every turn, heating and refluxing extraction 3 times, 1.5h for the first time, twice each 1h in back soaks 20min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, and be settled to soup: the medicinal material envelope-bulk to weight ratio is 2:1, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, and the NaOH solution according to the ratio adding 1mol/L that adds 0.01gNaOH in the 1g medicinal material is heated to 100 ℃, stirs, and continuous backflow 6h to 0.1g medicinal material/ml, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: according to the medicinal material amount: the amount of resin weight ratio is that 2:1 takes by weighing the HPD722 resin, and the blade diameter length ratio of packing into is the chromatography column of 1:3, with 95% ethanol and zero(ppm) water processing totally; With on the alkaline hydrolyzate appearance, absorption flow velocity be 6 times of column volumes/hour, saturated 1h; Carry out wash-out with the zero(ppm) water of 10 times of column volumes and remove sugar, elution flow rate be 12 times of column volumes/hour; With the NaOH solution removal of impurities of 10 times of column volume 0.1mol/L, elution flow rate be 12 times of column volumes/hour, dash to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 7 times of column volumes 40%, elution flow rate be 12 times of column volumes/hour; Ethanolic soln with 15 times of column volumes 60% carries out wash-out, elution flow rate be 12 times of column volumes/hour, collect 60% ethanol eluate, refined solution A;
D, purifying for the second time: according to the medicinal material amount: the amount of resin weight ratio is that 3.2:1 takes by weighing 330 weakly basic anion exchange resins, and the blade diameter length ratio of packing into is the chromatography column of 1:3, uses the acid-alkali treatment weakly basic anion exchange resin, and finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, flow velocity be 3.6 times of column volumes/hour, collect effluent; Flow through the weak anion resin post with 3 times of column volume 60% ethanolic solns, collect effluent; Two-part effluent merging is concentrated into 6.4g medicinal material/ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
The present invention extracts the Latin formal name used at school of the raw materials of traditional Chinese medicinal materials Radix Astragali in the method for refining astragalus first glycosides from the Radix Astragali: ASTRAGALI RADIX is the dry root of leguminous plants Radix Astagali Astragalus membranaceus (Fisch.) Bge. var. mongholicus (Bge.) Hsiao or Radix Astragali Astragalus membranaceus (Fisch.) Bge..
Solvent load in the leaching process of the present invention is certain doubly amount of medicinal material, and " doubly amount " described here is meant the weightmeasurement ratio of medicinal material and solvent, is that per kilogram Radix Astragali medicine materical crude slice adds 6L60% ethanol such as " 6 times of amount 60% ethanol ", and the volume of solvent is the normal temperature volume; The multiple of the column volume in the purge process also is meant the normal temperature volume.
Adopt the present invention from the Radix Astragali, to extract the method for refining astragalus first glycosides, produce five batches of Cyclosiversioside Fs according to the continuous parameters of embodiment 1, yield is more than 0.077%, and purity is more than 99%.Detailed results is seen table 1
Continuous five crowdes of purity and the rate of transform results that produce Cyclosiversioside F of table 1
| Lot number | Content % | Yield % |
| 081026 | 99.1 | 0.085 |
| 081117 | 99.5 | 0.077 |
| 081204 | 99.0 | 0.078 |
| 081220 | 99.1 | 0.084 |
| 090209 | 99.3 | 0.082 |
This shows, process for purification of the present invention, process stabilizing is reliable, is easy to suitability for industrialized production, produces purity more than 99%, the Cyclosiversioside F of yield more than 0.07%.And have the following advantages:
This production technique is simple, and is pollution-free, is suitable for big production; And the target compound that obtains is of light color, purity and yield are all higher.
Embodiment
Following embodiment is used for illustrating the method for the present invention from Radix Astragali extraction refining astragalus first glycosides, but it can not constitute any restriction to scope of the present invention.
Embodiment 1:
A, extraction: take by weighing Radix Astragali medicine materical crude slice 20kg, add the 240L80% ethanolic soln at every turn, heating and refluxing extraction 2 times, each 3h soaks 20min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, is settled to 40L, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, add the NaOH solution of 2.5L 1mol/L, be heated to 60 ℃, stir, continuous backflow 6h to 50L, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: take by weighing AB-8 resin 10kg, the diameter of packing into is 20 cm, highly is 60 cm, and volume is the chromatography column of 19L, with 95% ethanol and zero(ppm) water processing totally; With appearance on the alkaline hydrolyzate, the absorption flow velocity is 114L/h, saturated 3h; Zero(ppm) water with 380L carries out wash-out except that sugar, and elution flow rate is 228L/h; With the NaOH solution removal of impurities of 190L0.1mol/L, elution flow rate is 228L/h, dashes to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 133L40%, elution flow rate is 228L/h; Ethanolic soln with 190L 60% carries out wash-out, and elution flow rate is 228L/h, collects 60% ethanol eluate, gets refined solution A;
D, purifying for the second time: take by weighing D311 weakly basic anion exchange resin 6.25kg, the diameter of packing into is 11cm, highly is 111cm, and volume is the chromatography column of 10.6L, uses the acid-alkali treatment weakly basic anion exchange resin, and finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, and flow velocity is 38.2L/h, collects effluent; Flow through the weak anion resin post with the 53L60% ethanolic soln, collect effluent; Two-part effluent merging is concentrated into 1250ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
The result: get Cyclosiversioside F 15.4g, content is 99.1%, and yield is 0.077%.
Embodiment 2:
A, extraction: take by weighing Radix Astragali medicine materical crude slice 5kg, add the 30L60% ethanolic soln at every turn, heating and refluxing extraction 3 times, each 1h soaks 40min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, is settled to 5L, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, add the NaOH solution of 2.5L1mol/L, be heated to 100 ℃, stir, continuous backflow 2h to 12.5L, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: take by weighing macroporous adsorbent resin HPD100 resin 10kg, the diameter of packing into is 13cm, highly be 143cm, and volume is the chromatography column of 19L, with 95% ethanol and zero(ppm) water processing totally; With appearance on the alkaline hydrolyzate, the absorption flow velocity is 114L/h, saturated 1h; Zero(ppm) water with 190L carries out wash-out except that sugar, and elution flow rate is 228L/h; With the NaOH solution removal of impurities of 380L0.1mol/L, elution flow rate is 228L/h, dashes to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 133L40%, elution flow rate is 228L/h; Ethanolic soln with 380L60% carries out wash-out, and elution flow rate is 228L/h, collects 60% ethanol eluate, gets refined solution A;
D, purifying for the second time: take by weighing 5Kg weakly basic anion exchange resin D301 resin, the diameter of packing into is 15.5cm, highly is 46cm, and volume is the chromatography column of 8.7L, uses the acid-alkali treatment weakly basic anion exchange resin, and finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, and flow velocity is 31.3L, collects effluent; Flow through the weak anion resin post with the 26.1L60% ethanolic soln, collect effluent; Two-part effluent merging is concentrated into 780ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
The result: get Cyclosiversioside F 4.05g, content is 99.0%, and yield is 0.081%.
Embodiment 3:
A, extraction: take by weighing Radix Astragali medicine materical crude slice 10kg, add the 90L70% ethanolic soln at every turn, heating and refluxing extraction 3 times, each 2h soaks 30min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, is settled to 15L, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, add the NaOH solution of 3.75L 1mol/L, be heated to 80 ℃, stir, continuous backflow 4h to 41.7L, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: take by weighing 10kg macroporous adsorbent resin HPD910 resin, the diameter of packing into is 15cm, highly be 113cm, and volume is the chromatography column of 20L, with 95% ethanol and zero(ppm) water processing totally; With appearance on the alkaline hydrolyzate, the absorption flow velocity is 120L/h, saturated 2h; Zero(ppm) water with 300L carries out wash-out except that sugar, and elution flow rate is 240L/h; With the NaOH solution removal of impurities of 300L0.1mol/L, elution flow rate is 240L/h, dashes to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 140L40%, elution flow rate is 240L/h; Ethanolic soln with 300L60% carries out wash-out, and elution flow rate is 240L/h, collects 60% ethanol eluate, gets refined solution A;
D, purifying for the second time: take by weighing 21Kg weakly basic anion exchange resin D900 resin; The diameter of packing into is 11.8cm, highly is 76.7cm, and volume is the chromatography column of 8.3 L; Use the acid-alkali treatment weakly basic anion exchange resin, finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, and flow velocity is 30L/h, collects effluent; Flow through the weak anion resin post with the 33.2L60% ethanolic soln, collect effluent; Two-part effluent merging is concentrated into 892.8ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
The result: get Cyclosiversioside F 7.9g, content is 99.3%, and yield is 0.079%.
Embodiment 4:
A, extraction: take by weighing Radix Astragali medicine materical crude slice 15Kg, add the 120L80% ethanolic soln at every turn, heating and refluxing extraction 3 times, 1.5h first, twice each 1h in back soaks 20min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, is settled to 30L, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, add the NaOH solution of 3.75L1mol/L, be heated to 100 ℃, stir, continuous backflow 6h to 150L, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: take by weighing the 15KgHPD722 resin, the diameter of packing into is 18cm, highly be 54cm, and volume is the chromatography column of 15L, with 95% ethanol and zero(ppm) water processing totally; With appearance on the alkaline hydrolyzate, the absorption flow velocity is 90L/h, saturated 1h; Zero(ppm) water with 150L carries out wash-out except that sugar, and elution flow rate is 180L/h; With the NaOH solution removal of impurities of 150L0.1mol/L, elution flow rate is 180L/h, dashes to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 105L40%, elution flow rate is 180L/h; Ethanolic soln with 225L60% carries out wash-out, and elution flow rate is 180L/h, collects 60% ethanol eluate, gets refined solution A;
D, purifying for the second time: take by weighing the 4.69Kg330 weakly basic anion exchange resin, the diameter of packing into is 15.2cm, highly is 45.6cm, and volume is the chromatography column of 8.3 L, uses the acid-alkali treatment weakly basic anion exchange resin, and finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, and flow velocity is 30L/h, collects effluent; Flow through the weak anion resin post with the 25L60% ethanolic soln, collect effluent; Two-part effluent merging is concentrated into 2344ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
The result: get Cyclosiversioside F 12.45g, content is 99.4%, and yield is 0.083%.
Embodiment 5:
A, extraction: take by weighing Radix Astragali medicine materical crude slice 10kg, add the 90L70% ethanolic soln at every turn, heating and refluxing extraction 3 times, each 2h soaks 30min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, is settled to 15L, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, add the NaOH solution of 3.75L1mol/L, be heated to 80 ℃, stir, continuous backflow 4h to 41.7L, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: take by weighing 10kg macroporous adsorbent resin D101 resin, the diameter of packing into is 15cm, highly be 113cm, and volume is the chromatography column of 20L, with 95% ethanol and zero(ppm) water processing totally; With appearance on the alkaline hydrolyzate, the absorption flow velocity is 120L/h, saturated 2h; Zero(ppm) water with 300L carries out wash-out except that sugar, and elution flow rate is 240L/h; With the NaOH solution removal of impurities of 300L0.1mol/L, elution flow rate is 240L/h, dashes to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 140L40%, elution flow rate is 240L/h; Ethanolic soln with 300L60% carries out wash-out, and elution flow rate is 240L/h, collects 60% ethanol eluate, gets refined solution A;
D, purifying for the second time: take by weighing 21Kg weakly basic anion exchange resin 330 resins, the diameter of packing into is 11.8cm, highly is 76.7cm, and volume is the chromatography column of 8.3 L, uses the acid-alkali treatment weakly basic anion exchange resin, and finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, and flow velocity is 30L/h, collects effluent; Flow through the weak anion resin post with the 33.2L60% ethanolic soln, collect effluent; Two-part effluent merging is concentrated into 892.8ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
The result: get Cyclosiversioside F 8.1g, content is 99.1%, and yield is 0.081%.
Claims (6)
1. method of from the Radix Astragali, extracting refining astragalus first glycosides, this method comprises the steps:
A, extraction: take by weighing Radix Astragali medicine materical crude slice, add 6-12 at every turn and doubly measure the 60%-80% ethanolic soln, heating and refluxing extraction 2-3 time, each 1h-3h soaks 20min-40min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, and be settled to soup: the medicinal material envelope-bulk to weight ratio is 1:1-2:1, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, and the NaOH solution according to the ratio adding 1mol/L that adds 0.005g-0.02gNaOH in the 1g medicinal material is heated to 60 ℃-100 ℃; Stir; Continuous backflow 2h-6h to 0.04-0.4g medicinal material/ml, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: according to the medicinal material amount: the amount of resin weight ratio is that 2:1-1:2 takes by weighing macroporous adsorbent resin, and the blade diameter length ratio of packing into is the chromatography column of 1:3-1:12, with 95% ethanol and zero(ppm) water processing totally; With on the alkaline hydrolyzate appearance, absorption flow velocity be 6 times of column volumes/hour, saturated 1h-3h; Carry out wash-out with the zero(ppm) water of 10 times of-20 times of column volumes and remove sugar, elution flow rate be 12 times of column volumes/hour; With the NaOH solution removal of impurities of 10 times of-20 times of column volume 0.1mol/L, elution flow rate be 12 times of column volumes/hour, dash to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 7 times of column volumes 40%, elution flow rate be 12 times of column volumes/hour; Ethanolic soln with 10 times of-20 times of column volumes 60% carries out wash-out, elution flow rate be 12 times of column volumes/hour, collect 60% ethanol eluate, refined solution A;
D, purifying for the second time: according to the medicinal material amount: the amount of resin weight ratio is that 3.2:1-1:1 takes by weighing weakly basic anion exchange resin; The blade diameter length ratio of packing into is the chromatography column of 1:3-1:10; Use the acid-alkali treatment weakly basic anion exchange resin, finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, flow velocity be 3.6 times of column volumes/hour, collect effluent; Flow through the weak anion resin post with 3 times of-5 times of column volume 60% ethanolic solns, collect effluent; Two-part effluent merging is concentrated into 6.4g medicinal material/ml-16g medicinal material/ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
2. the method for from the Radix Astragali, extracting refining astragalus first glycosides according to claim 1 is characterized in that this method comprises the steps:
A, extraction: take by weighing Radix Astragali medicine materical crude slice, add 12 times of amount 80% ethanolic solns at every turn, heating and refluxing extraction 2 times, each 3h soaks 20min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, and be settled to soup: the medicinal material envelope-bulk to weight ratio is 2:1, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, and the NaOH solution according to the ratio adding 1mol/L that adds 0.005gNaOH in the 1g medicinal material is heated to 60 ℃, stirs, and continuous backflow 6h to 0.4g medicinal material/ml, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: according to the medicinal material amount: the amount of resin weight ratio is that 2:1 takes by weighing macroporous adsorbent resin, and the blade diameter length ratio of packing into is the chromatography column of 1:3, with 95% ethanol and zero(ppm) water processing totally; With on the alkaline hydrolyzate appearance, absorption flow velocity be 6 times of column volumes/hour, saturated 3h; Carry out wash-out with the zero(ppm) water of 20 times of column volumes and remove sugar, elution flow rate be 12 times of column volumes/hour; With the NaOH solution removal of impurities of 10 times of column volume 0.1mol/L, elution flow rate be 12 times of column volumes/hour, dash to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 7 times of column volumes 40%, elution flow rate be 12 times of column volumes/hour; Ethanolic soln with 10 times of column volumes 60% carries out wash-out, elution flow rate be 12 times of column volumes/hour, collect 60% ethanol eluate, refined solution A;
D, purifying for the second time: according to the medicinal material amount: the amount of resin weight ratio is that 3.2:1 takes by weighing weakly basic anion exchange resin, and the blade diameter length ratio of packing into is the chromatography column of 1:10, uses the acid-alkali treatment weakly basic anion exchange resin, and finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, flow velocity be 3.6 times of column volumes/hour, collect effluent; Flow through the weak anion resin post with 5 times of column volume 60% ethanolic solns, collect effluent; Two-part effluent merging is concentrated into 16g medicinal material/ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
3. the method for from the Radix Astragali, extracting refining astragalus first glycosides according to claim 1 is characterized in that this method comprises the steps:
A, extraction: take by weighing Radix Astragali medicine materical crude slice, add 6 times of amount 60% ethanolic solns at every turn, heating and refluxing extraction 3 times, each 1h soaks 40min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, and be settled to soup: the medicinal material envelope-bulk to weight ratio is 1:1, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, and the NaOH solution according to the ratio adding 1mol/L that adds 0.02gNaOH in the 1g medicinal material is heated to 100 ℃, stirs, and continuous backflow 2h to 0.04g medicinal material/ml, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: according to the medicinal material amount: the amount of resin weight ratio is that 1:2 takes by weighing macroporous adsorbent resin, and the blade diameter length ratio of packing into is the chromatography column of 1:12, with 95% ethanol and zero(ppm) water processing totally; With on the alkaline hydrolyzate appearance, absorption flow velocity be 6 times of column volumes/hour, saturated 1h; Carry out wash-out with the zero(ppm) water of 10 times of column volumes and remove sugar, elution flow rate be 12 times of column volumes/hour; With the NaOH solution removal of impurities of 20 times of column volume 0.1mol/L, elution flow rate be 12 times of column volumes/hour, dash to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 7 times of column volumes 40%, elution flow rate be 12 times of column volumes/hour; Ethanolic soln with 20 times of column volumes 60% carries out wash-out, elution flow rate be 12 times of column volumes/hour, collect 60% ethanol eluate, refined solution A;
D, purifying for the second time: according to the medicinal material amount: the amount of resin weight ratio is that 1:1 takes by weighing weakly basic anion exchange resin, and the blade diameter length ratio of packing into is the chromatography column of 1:3, uses the acid-alkali treatment weakly basic anion exchange resin, and finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, flow velocity be 3.6 times of column volumes/hour, collect effluent; Flow through the weak anion resin post with 3 times of column volume 60% ethanolic solns, collect effluent; Two-part effluent merging is concentrated into 6.4g medicinal material/ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
4. the method for from the Radix Astragali, extracting refining astragalus first glycosides according to claim 1 is characterized in that this method comprises the steps:
A, extraction: take by weighing Radix Astragali medicine materical crude slice, add 9 times of amount 70% ethanolic solns at every turn, heating and refluxing extraction 3 times, each 2h soaks 30min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, and be settled to soup: the medicinal material envelope-bulk to weight ratio is 1.5:1, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, and the NaOH solution according to the ratio adding 1mol/L that adds 0.015gNaOH in the 1g medicinal material is heated to 80 ℃, stirs, and continuous backflow 4h to 0.24g medicinal material/ml, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: according to the medicinal material amount: the amount of resin weight ratio is that 1:1 takes by weighing macroporous adsorbent resin, and the blade diameter length ratio of packing into is the chromatography column of 2:15, with 95% ethanol and zero(ppm) water processing totally; With on the alkaline hydrolyzate appearance, absorption flow velocity be 6 times of column volumes/hour, saturated 2h; Carry out wash-out with the zero(ppm) water of 15 times of column volumes and remove sugar, elution flow rate be 12 times of column volumes/hour; With the NaOH solution removal of impurities of 15 times of column volume 0.1mol/L, elution flow rate be 12 times of column volumes/hour, dash to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 7 times of column volumes 40%, elution flow rate be 12 times of column volumes/hour; Ethanolic soln with 15 times of column volumes 60% carries out wash-out, elution flow rate be 12 times of column volumes/hour, collect 60% ethanol eluate, refined solution A;
D, purifying for the second time: according to the medicinal material amount: the amount of resin weight ratio is that 2.1:1 takes by weighing weakly basic anion exchange resin, and the blade diameter length ratio of packing into is the chromatography column of 2:13, uses the acid-alkali treatment weakly basic anion exchange resin, and finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, flow velocity be 3.6 times of column volumes/hour, collect effluent; Flow through the weak anion resin post with 4 times of column volume 60% ethanolic solns, collect effluent; Two-part effluent merging is concentrated into 11.2g medicinal material/ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
5. according to each described method of from the Radix Astragali, extracting refining astragalus first glycosides of claim 1-4; It is characterized in that said macroporous adsorbent resin is a kind of in HPD722, HPD100, HPD910, AB-8, the D101 resin, said weak-base ion-exchange resin 330 resins.
6. the method for from the Radix Astragali, extracting refining astragalus first glycosides according to claim 1 is characterized in that comprising the steps:
A, extraction: take by weighing Radix Astragali medicine materical crude slice, add 8 times of amount 80% ethanolic solns at every turn, heating and refluxing extraction 3 times, 1.5h for the first time, twice each 1h in back soaks 20min first, filters; The filtrating of extraction merges, and being evaporated to does not have the alcohol flavor, and be settled to soup: the medicinal material envelope-bulk to weight ratio is 2:1, gets liquid concentrator;
B, basic hydrolysis: liquid concentrator is added in the extractor, and the NaOH solution according to the ratio adding 1mol/L that adds 0.01gNaOH in the 1g medicinal material is heated to 100 ℃, stirs, and continuous backflow 6h to 0.1g medicinal material/ml, gets alkaline hydrolyzate with distilled water diluting;
C, purifying for the first time: according to the medicinal material amount: the amount of resin weight ratio is that 2:1 takes by weighing the HPD722 resin, and the blade diameter length ratio of packing into is the chromatography column of 1:3, with 95% ethanol and zero(ppm) water processing totally; With on the alkaline hydrolyzate appearance, absorption flow velocity be 6 times of column volumes/hour, saturated 1h; Carry out wash-out with the zero(ppm) water of 10 times of column volumes and remove sugar, elution flow rate be 12 times of column volumes/hour; With the NaOH solution removal of impurities of 10 times of column volume 0.1mol/L, elution flow rate be 12 times of column volumes/hour, dash to neutral with zero(ppm) water; With the ethanolic soln removal of impurities of 7 times of column volumes 40%, elution flow rate be 12 times of column volumes/hour; Ethanolic soln with 15 times of column volumes 60% carries out wash-out, elution flow rate be 12 times of column volumes/hour, collect 60% ethanol eluate, refined solution A;
D, purifying for the second time: according to the medicinal material amount: the amount of resin weight ratio is that 3.2:1 takes by weighing 330 weakly basic anion exchange resins, and the blade diameter length ratio of packing into is the chromatography column of 1:3, uses the acid-alkali treatment weakly basic anion exchange resin, and finally using distilled water flushing to pH value is 7; Refined solution A is flow through the weakly basic anion exchange resin bed, flow velocity be 3.6 times of column volumes/hour, collect effluent; Flow through the weak anion resin post with 3 times of column volume 60% ethanolic solns, collect effluent; Two-part effluent merging is concentrated into 6.4g medicinal material/ml, gets refined solution B;
E, refining: refined solution B was placed in the refrigerator three days, filter then, filter cake changes with zero(ppm) water and dissolves the back freeze-drying, and it is dry that the sample after the freeze-drying is put into vacuum drier, and 95% ethyl alcohol recrystallization promptly gets Cyclosiversioside F.
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