CN104327079A - Method for extracting theophylline by using styrene-divinylbenzene copolymer resin - Google Patents
Method for extracting theophylline by using styrene-divinylbenzene copolymer resin Download PDFInfo
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- CN104327079A CN104327079A CN201410610978.XA CN201410610978A CN104327079A CN 104327079 A CN104327079 A CN 104327079A CN 201410610978 A CN201410610978 A CN 201410610978A CN 104327079 A CN104327079 A CN 104327079A
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- Prior art keywords
- theophylline
- styrene
- copolymer resin
- divinylbenzene copolymer
- extracts
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D473/00—Heterocyclic compounds containing purine ring systems
- C07D473/02—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6
- C07D473/04—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms
- C07D473/06—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3
- C07D473/08—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3 with methyl radicals in positions 1 and 3, e.g. theophylline
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/18—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
- B01D15/1814—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns recycling of the fraction to be distributed
- B01D15/1821—Simulated moving beds
- B01D15/185—Simulated moving beds characterized by the components to be separated
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/265—Adsorption chromatography
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention provides a method for extracting theophylline by using styrene-divinylbenzene copolymer resin. The method comprises the following steps: A, extraction of theophylline: preparing a chlorine salt solution, and soaking a tea medicinal material by using the chlorine salt solution for extraction; B, enrichment of theophylline: performing column chromatography and adsorption on an extracting solution by using macro-porous styrene-divinylbenzene copolymer resin, performing elution after adsorption, collecting an eluent, and then performing reduced pressure concentration to obtain an extract; and C, purification: performing alumina column chromatography on the extract, then performing elution, collecting the eluent, then performing reduced pressure concentration, and performing refrigeration, crystallization, filtration and drying on a concentrated solution to obtain theophylline compounds. According to the method provided by the invention, a large amount of high-quality theophylline compounds can be obtained by virtue of four steps namely acidic chlorine salt solution extraction, macroporous adsorption resin enrichment, alumina column chromatography and crystallization. The four steps are mild in condition, high in efficiency and short in preparation cycle; and the method is simple in technological process and simple and convenient to operate, has low requirements for the technological level of operators, and is suitable for industrial popularization.
Description
Technical field
The present invention relates to a kind of method that styrene-divinylbenzene copolymer resin extracts theophylline, belong to field of deep tea processing technology.
Background technology
Theophylline is methyl purine compounds, is the important component in tealeaves, and it has the effect of promotion central nervous excitation, and can also distend the blood vessels, accelerate blood circulation, strengthen muscle contractility, has effect of cardiac stimulant.It or one well diuretic(s), can strengthen renal function, unobstructed urine, the toxin in kidney and refuse are excreted as early as possible, so tealeaves can prevent nephropathy and lithiasis again.The effect mainly dissolved fat of theophylline, having helps digestion separates greasy effect.Drink tea and why can lose weight, and effectiveness comparison is remarkable, reason also here.Therefore, the extracting and developing process exploitation of highly purified theophylline, has great importance.Yet there are no the report of theophylline process of preparing in tealeaves.
Summary of the invention
The first object of the present invention is for the deficiencies in the prior art, provides a kind of styrene-divinylbenzene copolymer resin to extract the method for theophylline, the preparation cost of the method is low, the cycle is short, easy and simple to handle, obtained product purity is high.
For realizing the object of the invention, the technical scheme adopted is:
Styrene-divinylbenzene copolymer resin extracts a method for theophylline, comprises the following steps:
A. the extraction of theophylline: preparation chloride solution, by tealeaves medicinal material chloride solution soak extraction;
B. the enrichment of theophylline: by said extracted liquid Macroporous styrene-divinybenzene copolymers resin column chromatographic adsorption, wash-out after absorption, collect elutriant, then concentrating under reduced pressure obtains medicinal extract;
C. purifying: by medicinal extract by alumina column chromatography, then wash-out, collects elutriant, then concentrating under reduced pressure, and concentrated solution, through refrigeration, crystallization, filtration drying, obtains theophylline compounds;
The making step of described Macroporous styrene-divinybenzene copolymers resin is: vinylbenzene and divinylbenzene, liquid wax, BPO are mixed, and stirring heating reaction 10-12h, washing is dried rear surname extraction and get final product.
Further,
In step A, chloride solution massfraction is the 3.0-5.0% aqueous solution, and pH value is adjusted to 2-4; Soak extraction process is by the chloride solution soak extraction of the tealeaves medicinal material 8-10 times of volume of drying, and extract twice, each 48h, united extraction liquid, abandons the dregs of a decoction.
The making step of described Macroporous styrene-divinybenzene copolymers resin is: vinylbenzene and divinylbenzene, liquid wax, BPO are mixed, organic phase mixing solutions is suspended in be equivalent to organic phase quality 5 times containing 0.5% polyvinyl alcohol aqueous phase in, stirring heating reaction 10h, washing is dried rear surname extraction and get final product.
In step B, Macroporous styrene-divinybenzene copolymers resin volume with dry tealeaves part by weight is
1L-2L:1Kg.
The making step of described Macroporous styrene-divinybenzene copolymers resin is: vinylbenzene and divinylbenzene, liquid wax, BPO are mixed, organic phase mixing solutions is suspended in be equivalent to organic phase quality 5-6 doubly containing in the aqueous phase of 0.5%-0.7% polyvinyl alcohol, stirring heating reaction 10-12h, washing is dried rear surname extraction and get final product.
The wash-out of step B is the water elution removal of impurities first using 1.0BV, then uses the hydrophilic solvent wash-out of 2.5BV-4.0BV.
Step B is at 60 DEG C of-75 DEG C of concentrating under reduced pressure.
In step C, the weight ratio of medicinal extract and aluminum oxide is 1:(8-12).
Step C wash-out first adopts 4.0BV-6.0BV methylene chloride-methanol system wash-out, and in methylene chloride-methanol system, the volume ratio of methylene dichloride and methyl alcohol is 9-7:1-3, then adopts 16.0BV-20.0BV methanol-eluted fractions, merges meoh eluate.
The elutriant of step C carries out concentrating under reduced pressure in 45 DEG C-60 DEG C, and the concentrated solution volume after concentrated is the 1/12-1/8 of effluent volume.
Step C concentrated solution places 36h-48h, crystallization, filtration drying under putting refrigerator 4 DEG C of conditions, obtains the theophylline compounds that purity is greater than more than 80%.
Further,
When regulating chloride solution pH value, the acid adopted is one or more the mixture in hydrochloric acid, sulfuric acid, nitric acid; Villaumite in described steps A is NaCl, KCl or CaCl
2one or more mixture; Hydrophilic solvent in described step B is one or more mixture of methyl alcohol, acetone, ethanol.
hinge structure of the present invention has following advantage and effect:
One, the present invention compares ordinary polystyrene resin and has better adsorption effect, and can recycle.
Two, the present invention is by the lixiviate of acid chlorine salts solution, macroporous adsorbing resin for purification, alumina column chromatography, and crystallization four steps can obtain the theophylline compounds of a large amount of high-quality.The mild condition of four steps, require low, preparation cycle is short; Technical process is simple, easy and simple to handle, requires low to operator's state of the art, is applicable to industrialization promotion.
Embodiment
embodiment 1
The invention provides a kind of preparation method of theophylline, comprise the following steps:
(1) extraction of theophylline
Get dry theophylline 2kg, the massfraction preparing its 8 times of volumes is the KCl solution of 3.0%, and the pH value of chloride solution is adjusted to 2, and when regulating KCl solution ph, the acid adopted is hydrochloric acid, and extract 2 times, each 48h, united extraction liquid, abandons the dregs of a decoction;
(2) enrichment of theophylline
By united extraction liquid by Macroporous styrene-divinybenzene copolymers resin column chromatographic adsorption, macroporous adsorbent resin volume is 1Kg:1L with dry tealeaves medicinal material part by weight, and rate of adsorption controls at 2.0BV/h; After absorption, first use the water elution removal of impurities of 1.0BV; Use the hydrophilic solvent wash-out of 2.5BV again, described hydrophilic solvent is the ethanol of mass concentration 30%, collects elutriant, obtains medicinal extract in 60 DEG C of concentrating under reduced pressure;
(3) purifying
By medicinal extract by alumina column chromatography: the weight ratio of medicinal extract and filling alumina is 1:8, first adopt 4.0BV methylene chloride-methanol system wash-out, in methylene chloride-methanol system, the volume ratio of methylene dichloride and methyl alcohol is 9:1, then adopts 16.0BV methanol-eluted fractions, merges meoh eluate; The elutriant of methanol-eluted fractions is carried out concentrating under reduced pressure in 45 DEG C, makes the concentrated solution volume after concentrating be 1/12 of effluent volume, place 48h, crystallization, filtration drying under then concentrated solution being put refrigerator 4 DEG C of conditions, obtain theophylline monomer 5.1g.
Utilize reverse high performance liquid chromatography (RP-HPLC) to detect the theophylline purity of this example, recording its purity is 85%.
embodiment 2
A preparation method for theophylline monomer, comprises the following steps:
(1) the tealeaves 2kg of the extraction drying of theophylline, the massfraction preparing its 10 times of volumes is the NaCl solution of 4.0%, and the pH value of chloride solution is adjusted to 2.5, when regulating chloride solution pH value, the acid adopted is sulfuric acid, extracts 2 times, each 48h, united extraction liquid, abandons the dregs of a decoction;
(2) enrichment of theophylline
By united extraction liquid by Macroporous styrene-divinybenzene copolymers resin column chromatographic adsorption, macroporous adsorbent resin volume is 1Kg:2L with dry tealeaves part by weight, and rate of adsorption controls at 2.5BV/h; After absorption, first use the water elution removal of impurities of 1.0BV; Use the hydrophilic solvent wash-out of 3.0BV again, described hydrophilic solvent is 35% methyl alcohol, collects elutriant, obtains medicinal extract in 75 DEG C of concentrating under reduced pressure;
(3) purifying
By medicinal extract by alumina column chromatography: the weight ratio of medicinal extract and filling alumina is 1:12, first adopt 5.0BV methylene chloride-methanol system wash-out, in methylene chloride-methanol system, the volume ratio of methylene dichloride and methyl alcohol is 8:2, then adopts 18.0BV methanol-eluted fractions, merges meoh eluate; The elutriant of methanol-eluted fractions is carried out concentrating under reduced pressure in 60 DEG C, makes the concentrated solution volume after concentrating be 1/10 of effluent volume, place 36h, crystallization, filtration drying under then concentrated solution being put refrigerator 4 DEG C of conditions, obtain theophylline 5.0g.Utilize reverse high performance liquid chromatography (RP-HPLC) to detect the theophylline monomer purity of this example, recording its purity is 83%.
Claims (10)
1. styrene-divinylbenzene copolymer resin extracts a method for theophylline, it is characterized in that, comprises the following steps:
A. the extraction of theophylline: prepare chloride solution and adjust ph, by tealeaves medicinal material chloride solution soak extraction;
B. the enrichment of theophylline: by said extracted liquid Macroporous styrene-divinybenzene copolymers resin column chromatographic adsorption, wash-out after absorption, collect elutriant, then concentrating under reduced pressure obtains medicinal extract;
C. purifying: by medicinal extract by alumina column chromatography, then wash-out, collects elutriant, then concentrating under reduced pressure, and concentrated solution, through refrigeration, crystallization, filtration drying, obtains theophylline compounds;
The making step of described Macroporous styrene-divinybenzene copolymers resin is: vinylbenzene and divinylbenzene, liquid wax, BPO are mixed, and stirring heating reaction 10-12h, washing is dried rear surname extraction and get final product.
2. a kind of styrene-divinylbenzene copolymer resin according to claim 1 extracts the method for theophylline, it is characterized in that: in step A, chloride solution massfraction is the 3.0-5.0% aqueous solution, and pH value is adjusted to 2-4.
3. a kind of styrene-divinylbenzene copolymer resin according to claim 1 extracts the method for theophylline, it is characterized in that: the making step of described Macroporous styrene-divinybenzene copolymers resin is: vinylbenzene and divinylbenzene, liquid wax, BPO are mixed, organic phase mixing solutions is suspended in be equivalent to organic phase quality 5-6 doubly containing in the aqueous phase of 0.5%-0.7% polyvinyl alcohol, stirring heating reaction 10-12h, washing is dried rear surname extraction and get final product.
4. a kind of styrene-divinylbenzene copolymer resin according to claim 1 extracts the method for theophylline, it is characterized in that: in step A, soak extraction process is by the chloride solution soak extraction of the tealeaves medicinal material 8-10 times of volume of drying, extract twice, each 48h, united extraction liquid, abandons the dregs of a decoction.
5. a kind of styrene-divinylbenzene copolymer resin according to claim 1 extracts the method for theophylline, it is characterized in that: in step B, Macroporous styrene-divinybenzene copolymers resin volume is 1L-2L:1Kg with dry tealeaves part by weight.
6. a kind of styrene-divinylbenzene copolymer resin according to claim 1 extracts the method for theophylline, it is characterized in that: the wash-out of step B is the water elution removal of impurities first using 1.0BV, use the hydrophilic solvent wash-out of 2.5BV-4.0BV again, at 60 DEG C of-75 DEG C of concentrating under reduced pressure after wash-out.
7. a kind of styrene-divinylbenzene copolymer resin according to claim 1 extracts the method for theophylline, it is characterized in that: in step C, the weight ratio of medicinal extract and aluminum oxide is 1:(8-12).
8. a kind of styrene-divinylbenzene copolymer resin according to claim 1 extracts the method for theophylline, it is characterized in that: step C wash-out first adopts 4.0BV-6.0BV methylene chloride-methanol system wash-out, in methylene chloride-methanol system, the volume ratio of methylene dichloride and methyl alcohol is 9-7:1-3, adopt 16.0BV-20.0BV methanol-eluted fractions again, merge meoh eluate; Elutriant carries out concentrating under reduced pressure in 45 DEG C-60 DEG C, and the concentrated solution volume after concentrated is the 1/12-1/8 of effluent volume.
9. a kind of styrene-divinylbenzene copolymer resin according to claim 1 extracts the method for theophylline, it is characterized in that: step C concentrated solution places 36h-48h under putting refrigerator 4 DEG C of conditions, crystallization, filtration drying, obtains the theophylline compounds that purity is greater than more than 80%.
10. a kind of styrene-divinylbenzene copolymer resin according to claim 1 extracts the method for theophylline, it is characterized in that: when regulating chloride solution pH value, the acid adopted is one or more the mixture in hydrochloric acid, sulfuric acid, nitric acid; Villaumite in described steps A is NaCl, KCl or CaCl
2one or more mixture; Hydrophilic solvent in described step B is one or more mixture of methyl alcohol, acetone, ethanol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410610978.XA CN104327079A (en) | 2014-11-04 | 2014-11-04 | Method for extracting theophylline by using styrene-divinylbenzene copolymer resin |
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| CN103992321A (en) * | 2014-06-09 | 2014-08-20 | 成都合瑞化工有限公司 | Preparation method of theophylline |
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| CN103992321A (en) * | 2014-06-09 | 2014-08-20 | 成都合瑞化工有限公司 | Preparation method of theophylline |
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| CN109422747A (en) * | 2017-08-25 | 2019-03-05 | 仝丹丹 | A kind of preparation method of theophylline |
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Application publication date: 20150204 |