CN101108214B - Method of separating and extracting natural base from coptis chinensis with latex membrane - Google Patents
Method of separating and extracting natural base from coptis chinensis with latex membrane Download PDFInfo
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- CN101108214B CN101108214B CN200710035399A CN200710035399A CN101108214B CN 101108214 B CN101108214 B CN 101108214B CN 200710035399 A CN200710035399 A CN 200710035399A CN 200710035399 A CN200710035399 A CN 200710035399A CN 101108214 B CN101108214 B CN 101108214B
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Abstract
The invention discloses a method for extracting alkaloid in Chinese goldthread coptis through separating emulsion liquid membrane. The emulsion is prepared by taking cooking oil as the membrane solvent, the Span 80 or the mixture of the Span 80 and the cosurfactant as the surface active agent and the phosphate ester as the carrier. Adding the Chinese goldthread coptis hydrochloric acid extractionliquid or vitriol extraction liquid with the pH value equals to 4 and the emulsion with the volume ratio between water and the emulsion as (50:5 to 50:20); stiring with low speed of 200 times per minsto 300 times per mins for extracting for 5 to 15 min; separating out the oil layer after breaking the emulsion through heating in water and the water obtained is just the solution of the total alkaloid in the Chinese goldthread coptis. The invention, by taking the cooking oil as the membrane solvent, resolves the difficulty that the organic solvent used for the existing emulsion membrane is venomous and is unsuitable being used for human and animal after extracted the Chinese medicinal herb, has the advantages of speedy extraction, high efficiency and simple operation, which is applied for producing, developing and inspecting the Chinese goldthread coptis medicine and veterinary medicine.
Description
Technical field
The present invention relates to alkaloidal method in a kind of emulsion liquid film separation and Extraction coptis that can be applicable to medicinal material production and Pharmaceutical Analysis check.
Background technology
The coptis belongs to the Mao Moke plant, is a kind of Chinese medicine of having many uses, medicinal its dry rhizome of getting, and main medicinal ingredient is alkaloids such as jamaicin, jateorrhizine, palmatine.They have analog structure, often are referred to as coptis alkaloid.Extracting method commonly used is a reflux extraction, as ethanol water refluxing extraction or water refluxing extraction.This technology gained finished product is impure more, needs to improve by recrystallization the purity of finished product, yet recrystallization causes the loss of coptis chinensis total alkaloid again inevitably.02103880.5 disclose " a kind of extraction process of coptis chinensis total alkaloid ", be earlier with coptis fragmentation, the water logging bubble also carries out the ultrasonic wave processing simultaneously then, water-soaking time is 30～240 minutes, the coptis behind the water logging bubble is soaked in temperature and carries out the TA extraction under the condition, extracting temperature is 70～98 ℃, the amount of aqueous solvent is 5～16 times of raw medicinal herbs weight during extraction, extraction time is 30～180 minutes, extraction time is 1～4 time, it is concentrated extract to be reduced pressure again, vacuum when concentrating is 0.04～0.08MPa, the volume of the water of concentrated extracting solution to 2～10 times raw medicinal herbs weight with pH value to 1～5 of concentrated hydrochloric acid adjusting concentrated extracting solution, adds 4%～16% sodium chloride again and dissolves while hot then, concentrated extracting solution left standstill 4～24 hours, by the sediment in suction filtration or the centrifuge dripping collection extract, sediment is dried under 50～80 ℃ temperature, and dried sediment is pulverized can obtain coptis chinensis total alkaloid hydrochloride finished product.This method complex operation, time-consuming, consumption of raw materials is many.Emulsion liquid membrane be a kind of simple, fast, efficient, selectivity is high, the novel separation and extraction technology of economical and energy saving, fields such as environment, Chemical Manufacture, hydrometallurgy have been applied to, but also be not applied to the extraction of TA in the Chinese herbal medicine, and the membrane solvent of existing emulsion liquid film normally toluene, cyclohexane, carrene and kerosene; These solvents all have certain toxicity, are not suitable for the use that Chinese herbal medicine extracts the back people, animal.
Summary of the invention
The object of the present invention is to provide alkaloidal method in a kind of liquid film separation and Extraction coptis.To realize that leaching process is quick, efficient, simple to operate and selected solvent is nontoxic, can be suitable for people, animal use after the pharmacy.
The present invention includes following steps:
(1) preparation of emulsion: by membrane solvent edible oil: surfactant Span 80 or Span 80 mixture with cosurfactant: the volume ratio of phosphoric acid fat carrier=(31～45): (3～9): mix (2～10), adding concentration by 1: 1～4: 1 volume ratios then in mixture is HCl solution or the dilution heat of sulfuric acid of 0.1～0.7mol/L, under 8000 rev/mins～10000 rev/mins rotating speed, stir 1-3min, promptly make stable w/o type emulsion;
(2) alkaloidal separation and Extraction: coptis hydrochloric acid extraction liquid and the emulsion of pH=4 are added in the extractor according to certain volume ratio (50: 5～50: 20), under 200 rev/mins～300 rev/mins stirring at low speed, extract 5-15min;
(3) breakdown of emulsion: change emulsion in separatory funnel standing demix, tell emulsion, divide oil-yielding stratum behind the water-bath heating demulsification type, the gained water is TA solution in the coptis.
The coptis hydrochloric acid extraction liquid of described pH=4 is in 1 part of Golden Thread, adds the HCl of 30-60 part 0.1mol/L, ultrasonic extraction secondary, each 50-70min, centrifugation uses the HCl of 0.1mol/L to dilute 8-10 doubly filtrate, regulates pH=4 with saturated NaOH again.
Described cosurfactant is that the C atomicity is the alcohols of 8-16, and surfactant Span 80 is 1: 6～7: 11 with the volume ratio of cosurfactant.
Described cosurfactant is a Decanol.
Described phosphoric acid fat carrier is a di-(2-ethylhexyl)phosphoric acid fat.
The present invention uses edible oil as membrane solvent, and it is poisonous to have solved the present employed organic solvent of emulsion liquid membrane, is not suitable for Chinese herbal medicine and extracts the difficult problem that the back people, animal uses; Leaching process is quick, efficient, simple to operate, can be applicable to production and the exploitation and the check of products such as coptis medicine, veterinary drug.
The specific embodiment
Below the invention will be further described by specific embodiment:
Embodiment 1:
(1) preparation of rhizoma extracting liquid: take by weighing 1.0 gram Golden Threads, the HCl that adds 50mL 0.1mol/L, ultrasonic extraction 60min, at rotating speed centrifugal 10min on the centrifuge of 4000r/min, take out filtrate, add the HCl of the 0.1mol/L of 50mL in the filter residue again, ultrasonic extraction 60min, centrifugal again 10min, merging filtrate.HCl with 0.1mol/L dilutes filtrate to 900mL, filters, and is with saturated NaOH adjustment pH=4, standby.
(2) preparation of emulsion: get membrane solvent edible oil 37mL, the surfactant total amount is 7mL, wherein Span 80 is 1mL, Decanol is 6mL, phosphoric acid fat carrier 6mL mixes the three, whenever gets this mixture 20mL just adds 10mL 0.1mol/L by 2: 1 volume ratio HCl solution, under 9000 rev/mins rotating speed, stir 2min, promptly make stable w/o type emulsion.
(3) alkaloidal separation and Extraction: is to add in extractor at 50: 10 the coptis hydrochloric acid extraction liquid of pH=4 and emulsion according to the whey volume ratio, extracts 10min 250 rev/mins stirring at low speed;
(4) breakdown of emulsion: change standing demix in the separatory funnel over to, tell emulsion, divide oil-yielding stratum behind the water-bath heating demulsification type, the gained water is the solution of TA in the coptis.
Through efficient liquid phase chromatographic analysis, the extraction yield of jateorrhizine, palmatine and jamaicin has reached 82.97%, 85.92% and 88.86% respectively; Its enrichment factor has reached 7.21,6.93 and 6.97 respectively, and the emulsion liquid film alkaloid in the separation and concentration coptis effectively is described.
The condition of high performance liquid chromatography is as follows:
Chromatographic column: Spherigel C18, SZ:200 * 4.6mm, 5 μ m
Phase flows: A (50mmol/LKH
2PO
4+ 14mmol/L triethylamine+3.6mmol/LC
12H
25NaO
3S): B (acetonitrile)=65: 35 (V/V)
Flow velocity: 1.0mL/min
Detect wavelength: 346nm
Sample size: 10 μ L
Column temperature: 30 ℃
Embodiment 2:
(1) preparation of rhizoma extracting liquid: take by weighing 2 kilograms of coptis extract powder, the HCl that adds 120L 0.1mol/L, ultrasonic extraction 70min, at rotating speed centrifugal 10min on the centrifuge of 4000r/min, take out filtrate, add the HCl of the 0.1mol/L of 120L in the filter residue again, ultrasonic extraction 70min, centrifugal again 10min, merging filtrate.HCl with 0.1mol/L dilutes filtrate to 2400L, filters, and is with saturated NaOH adjustment pH=4, standby;
(2) preparation of emulsion: get membrane solvent edible oil 124L, the surfactant total amount is 36L, wherein Span80 is 14L, Decanol is 22L, phosphoric acid fat carrier 40L mixes the three, then the HCl solution of this mixture and the 0.7mol/L volume ratio according to 4: 1 is added in the newborn device of system, under 10000 rev/mins rotating speed, stir 15min, promptly make stable w/o type emulsion.
(3) alkaloidal separation and Extraction: is to add in extractor at 50: 5 the coptis hydrochloric acid extraction liquid of pH=4 and emulsion according to the whey volume ratio, extracts 15min 300 rev/mins stirring at low speed;
(4) breakdown of emulsion: change standing demix in the separatory funnel over to, tell emulsion, divide oil-yielding stratum behind the water-bath heating demulsification type, the gained water is the solution of TA in the coptis, with efficient liquid phase chromatographic analysis wherein the separating of jateorrhizine, palmatine and jamaicin, enrichment degree.
Through efficient liquid phase chromatographic analysis, the extraction yield of jateorrhizine, palmatine and jamaicin has reached 72.85%, 78.22% and 82.08% respectively; Its enrichment factor has reached 6.65,6.51 and 6.82 respectively, and the emulsion liquid film alkaloid in the separation and concentration coptis effectively is described.
The condition of high performance liquid chromatography is as follows:
Chromatographic column: Spherigel C18, SZ:200 * 4.6mm, 5 μ m
Phase: A (50mmol/L KH flows
2PO
4+ 14mmol/L triethylamine+3.6mmol/LC
12H
25NaO
3S): B (acetonitrile)=65: 35 (V/V)
Flow velocity: 1.0mL/min
Detect wavelength: 346nm
Sample size: 10 μ L
Column temperature: 30 ℃
Embodiment 3:
(1) preparation of rhizoma extracting liquid: take by weighing 1.0 gram Golden Threads, the HCl that adds 30mL 0.1mol/L, ultrasonic extraction 30min, at rotating speed centrifugal 10min on the centrifuge of 4000r/min, take out filtrate, add the HCl of the 0.1mol/L of 30mL in the filter residue again, ultrasonic extraction 30min, centrifugal again 10min, merging filtrate.HCl with 0.1mol/L dilutes filtrate to 500mL, filters, and is with saturated NaOH adjustment pH=4, standby.
(2) preparation of emulsion: get membrane solvent edible oil 42mL, the surfactant total amount is 3.5mL, wherein Span 80 is 0.5mL, Decanol is 3mL, phosphoric acid fat carrier 4.5mL mixes the three, whenever gets this mixture 20mL just adds 20mL 0.4mol/L by 1: 1 volume ratio HCl solution, under 8000 rev/mins rotating speed, stir 1min, promptly make stable w/o type emulsion.
(3) alkaloidal separation and Extraction: is to add in extractor at 50: 20 the coptis hydrochloric acid extraction liquid of pH=4 and emulsion according to the whey volume ratio, extracts 5min 200 rev/mins stirring at low speed;
(4) breakdown of emulsion: change standing demix in the separatory funnel over to, tell emulsion, divide oil-yielding stratum behind the water-bath heating demulsification type, the gained water is the solution of TA in the coptis, with efficient liquid phase chromatographic analysis wherein the separating of jateorrhizine, palmatine and jamaicin, enrichment degree.
Through efficient liquid phase chromatographic analysis, the extraction yield of jateorrhizine, palmatine and jamaicin has reached 75.25%, 79.24% and 82.44% respectively; Its enrichment factor has reached 6.45,6.48 and 6.71 respectively, and the emulsion liquid film alkaloid in the separation and concentration coptis effectively is described.
Claims (4)
1. alkaloidal method in the emulsion liquid film separation and Extraction coptis is characterized in that may further comprise the steps:
(1) preparation of emulsion: by the mixture of membrane solvent edible oil: Span 80 with cosurfactant: volume ratio=31～45 of phosphoric acid fat carrier: 3～9: 2～10 mix, described cosurfactant is that the C atomicity is the alcohols of 8-16, and surfactant Span 80 is 1: 6～7: 11 with the volume ratio of cosurfactant; Adding concentration by 1: 1～4: 1 volume ratios then in mixture is HCl solution or the dilution heat of sulfuric acid of 0.1～0.7mol/L, stirs 1-3min under 8000 rev/mins～10000 rev/mins rotating speed, promptly makes stable w/o type emulsion;
(2) alkaloidal separation and Extraction: coptis hydrochloric acid extraction liquid and the emulsion of pH=4 were added in the extractor according to volume ratio in 50: 5～50: 20, under 200 rev/mins～300 rev/mins stirring at low speed, extract 5-15min;
(3) breakdown of emulsion: change emulsion in separatory funnel standing demix, tell emulsion, divide oil-yielding stratum behind the water-bath heating demulsification type, the gained water is TA solution in the coptis.
2. alkaloidal method in the emulsion liquid film separation and Extraction coptis according to claim 1, the coptis hydrochloric acid extraction liquid that it is characterized in that described pH=4 is in 1 part of Golden Thread, the HCl that adds 30-60 part 0.1mol/L, ultrasonic extraction secondary, each 50-70min, centrifugation uses the HCl of 0.1mol/L to dilute 8-10 doubly filtrate, regulates pH=4 with saturated NaOH again.
3. alkaloidal method in the emulsion liquid film separation and Extraction coptis according to claim 1 is characterized in that described cosurfactant is a Decanol.
4. alkaloidal method in the emulsion liquid film separation and Extraction coptis according to claim 1 is characterized in that, described phosphoric acid fat carrier is a di-(2-ethylhexyl)phosphoric acid fat.
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| DE102009040381A1 (en) * | 2009-09-07 | 2011-03-17 | Kallimopoulos, Thomas, Dr. | Process for the isolation of alkaloids from plants |
| CN103550322B (en) * | 2013-11-13 | 2015-09-30 | 西南大学 | The processing method of Rhizoma Coptidis |
| CN107903403B (en) * | 2017-12-13 | 2020-04-28 | 齐鲁工业大学 | Method for separating and extracting lignin in papermaking black liquor by magnetic emulsion liquid membrane |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450074A (en) * | 2002-04-05 | 2003-10-22 | 北京康思瞄医药技术开发有限公司 | Process for extracting coptis total alkaloid and new use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1450074A (en) * | 2002-04-05 | 2003-10-22 | 北京康思瞄医药技术开发有限公司 | Process for extracting coptis total alkaloid and new use thereof |
Non-Patent Citations (6)
| Title |
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| 梁锋等.乳状液膜分离提取荷叶中3种生物碱.精细化学第24卷 第6期.2007,第24卷(第6期),第565-570页. |
| 梁锋等.乳状液膜分离提取荷叶中3种生物碱.精细化学第24卷 第6期.2007,第24卷(第6期),第565-570页. * |
| 王大杰等.用液膜法从黄连中提取黄连素的研究.成都大学学报（自然科学版）第25卷 第4期.2006,第25卷(第4期),第260-262,266页. |
| 王大杰等.用液膜法从黄连中提取黄连素的研究.成都大学学报(自然科学版)第25卷 第4期.2006,第25卷(第4期),第260-262,266页. * |
| 马智兰等.正交实验法研究液膜提取黄连素的最佳条件.膜科学与技术第21卷 第1期.2001,第21卷(第1期),第56-58页. |
| 马智兰等.正交实验法研究液膜提取黄连素的最佳条件.膜科学与技术第21卷 第1期.2001,第21卷(第1期),第56-58页. * |
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