CN102258580A - Macleaya cordata total alkaloid preparation method - Google Patents
Macleaya cordata total alkaloid preparation method Download PDFInfo
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- CN102258580A CN102258580A CN2011101870836A CN201110187083A CN102258580A CN 102258580 A CN102258580 A CN 102258580A CN 2011101870836 A CN2011101870836 A CN 2011101870836A CN 201110187083 A CN201110187083 A CN 201110187083A CN 102258580 A CN102258580 A CN 102258580A
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Abstract
The invention discloses a macleaya cordata total alkaloid preparation method. According to the preparation method provided by the invention, technologies of supersonic-wave continuous countercurrent extraction, ceramic membrane purification, sodium filter membrane condensation, intelligent static microwave vacuum drying technology and the like are adopted to prepare the macleaya cordata extract so as to raise the extraction efficiency of macleaya cordata with one-time extraction rate being over 0.7-1%; in addition, the total alkaloid has high purity and good quality; the preparation technology is simple, the technology period is shortened, the energy consumption and production cost are reduced, there is no pollution during the technology process, and the preparation method is applicable to large-scale industrial cleaning production. Waste residues generated after the extraction of the macleaya cordata total alkaloid can be used as organic fertilizers or fuels for reutilization, thus leading to the full application and development of the macleaya cordata resource.
Description
Technical field
The present invention relates to the Chinese traditional medicine biology pharmaceutical field, specifically is a kind of method for preparing the Chinese medicine macleaya cordata total alkaloid.
Background technology
The Herba Macleayae Cordatae biology total alkali comes from the herb and the fruit pod of bloodroot Herba Macleayae Cordatae, belongs to the benzo phenanthridine alkaloid, has excellent antibiotic, antiinflammatory, parasite killing, kills the maggot function, and nervus centralis is had anesthetic action, in medicinal existing more than the 1000 year history of China.Discover both at home and abroad and Herba Macleayae Cordatae extract can be developed into antiviral people's veterinary drug thing and feed additive, organic parasite killing, antibacterial.Macleaya cordata total alkaloid is a kind of material with anti-inflammation, heat-clearing and toxic substances removing, anti-kinds of tumors, can pesticide-germicide, simultaneously also because the antibiotic and sterilizing effect of macleaya cordata total alkaloid, and being widely used in toothpaste, collutory, shampoo, skin protection facial cream, surgical operation is with in articles for daily use such as soap, disinfectant solution and the medical supplies.Mainly contain in the infruit of Herba Macleayae Cordatae extract and will contain the benzylisoquinoline total alkaloids, wherein comprise Sanguinarine, chelerythrine, protopine, allocryptopine, 13-methyl-13,14-dihydro-[1,3, dihydro allocryptopine etc.The natural antibiotics product that adopts modern medicine biological technique to produce to meet human needs is the needs of Development of Human Civilization, and more can not be at the cost of the environment when producing the natural antibiotics product.Existing Chinese medicine macleaya cordata total alkaloid extractive technique is to adopt following method to realize:
(1) Chinese medicine macleaya cordata total alkaloid extractive technique is the acid extraction that adopts, alkaline chemical precipitation, the leaching precipitation is with the precipitate organic solvent extraction, adopt the acid crystal salifying method again, the weak point of this technology can produce behind alkaline chemical precipitation and contain alkali organic wastewater in a large number.
(2) in disclosed technology, publication number CN 101020703A, it is to have taked ethanol step impregnation, ultrasonic Treatment extraction, macroporous resin separation and purification, microwave vacuum drying preparation method, and macroporous resin adsorbs when separating, just washes, desorbing, cleaning etc.
(3) publication number CN 101491587A, it is to have taked to get the Herba Macleayae Cordatae extracting solution, adjusts pH value 1 to 7, filter, get filtrate and be added on the cation exchange resin column, earlier with the water elution remove impurity, the saline solution with 0.5%-20% soaks resin column again, again to contain acid or alcoholic acid 0.5%-20% saline solution eluting, check and collect eluent till the inanimate object alkali, add the alkali neutralization, through desalting processing, concentrate drying gets the Chinese medicine macleaya cordata total alkaloid.
The yield that above method prepares macleaya cordata total alkaloid is generally 0.5-0.7%, all is lower than 0.7%.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing the Chinese medicine macleaya cordata total alkaloid; adopt modern technologies to realize organic production of Chinese medicine macleaya cordata total alkaloid; improved the Herba Macleayae Cordatae extraction efficiency; technology is comparatively easy; shortened process cycle, reduced energy consumption and production cost, technical process is pollution-free and be adapted to the large-scale industrial cleaner production.
The object of the present invention is achieved like this: infruit of Herba Macleayae Cordatae is pulverized, join in the ultrasound wave counterflow extraction apparatus, add extracting solution by the other end then and carry out the adverse current supersound extraction, add clarifier or precipitant precipitate and separate macromolecular substances in the extracting solution, reclaim organic solvent and be concentrated into and do not contain organic solvent and be made into 5% solution with pure water, adopt ceramic membrane ultrafitration purification, sodium filter membrane concentrate the Herba Macleayae Cordatae concentrated solution, obtain macleaya cordata total alkaloid through microwave vacuum drying.Specifically may further comprise the steps:
(1) the ultrasound wave adverse current is extracted continuously:
A, infruit of Herba Macleayae Cordatae is pulverized;
B, the infruit of Herba Macleayae Cordatae powder that will crush by solid-liquid ratio add in the continuous flow upstream ultrasonic device;
C, extracting solution is pumped into dosing pump at the equipment other end and to carry out the adverse current supersound extraction in the equipment;
D, extracting solution separate with dreg-liquid separator, and the waste residue behind the extraction macleaya cordata total alkaloid enters the organic solvent in the organic solvent recovery system recovery residue;
E, add 1-10% clarifier, filter aid in the extracting solution, remove precipitate through vacuum filtration, filtrate enters reclaims concentration systems and reclaims in the extracting solution organic solvent to not containing organic solvent, Herba Macleayae Cordatae crude extract aqueous solution dope;
(2), ceramic membrane separates
1.. get Herba Macleayae Cordatae crude extract aqueous solution coarse filtration (active carbon+quartz sand), three grades of doughnut membrane filtrations are removed mechanical admixture in the solution, enter micro-filtration membrane and carry out microfiltration;
2.. the Herba Macleayae Cordatae crude extract (by volume) behind the microfiltration is made into the 1-5% diluent with pure water, further removes macromolecular substances such as albumen, pigment, polysaccharide and inorganic salt, micromolecule pigment, monosaccharide and the ash micromolecule thing impurity that grades with the ceramic super-filtering film ultrafiltration;
(3) the sodium filter membrane concentrates
Herba Macleayae Cordatae essence extract liquid behind the ceramic membrane ultrafitration purification is concentrated into 5-20 ° of Be ' by the sodium filter membrane;
(4), Intelligentized static microwave vacuum drying
5-20 ° of Be ' concentrated solution used the drying machine drying at 20-50 ℃, and 〉=100 order jet mills are pulverized, and get product.
The grinding particle size scope of described Herba Macleayae Cordatae is 40 orders-60 orders.
Described extracting solution is that described solvent is to use pure water, also can be methanol, and ethanol, ethyl acetate are wherein a kind of.
Described supersonic frequency is that 30-60KHz, ultrasonic time are the 15-75 branch, ultrasonic power 12-76KW, and 50-80 ℃ of temperature of extraction, solid-liquid ratio are 1: 5.
Described clarifier is higher derivative, ZTC 1+1 natural clarifying agent, carrageenan, Bentonite (Bentonite), the crospovidone (PVPP) of silicon dioxide gel (Silica sol), chitosan; Filter aid is kieselguhr, silica flour, perlite, also can is Pulvis Talci.
Described ceramic super-filtering film adopts molecular cut off to purify for the 10000-30000 ceramic membrane.
Described sodium filter membrane concentrates, and adopts 500-1000 sodium filter membrane to concentrate.
Described drying machine is vacuum microwave drier, round vacuum microwave drier, square vacuum microwave drier, drying machine with centrifugal spray.
Innovative point of the present invention is: adopted physics extraction purification and sodium filter membrane concentration technique, the microwave vacuum cold drying technology of ultrasound wave and ultrafilter membrane purification to be applied to producing of Herba Macleayae Cordatae extract, improved the Herba Macleayae Cordatae extraction efficiency, one time extraction ratio can reach more than the 0.7-1%, and the purity height of total alkaloids, quality is good; Preparation technology is comparatively easy, has shortened process cycle, has reduced energy consumption and production cost, and technical process is pollution-free and be adapted to the large-scale industrial cleaner production.Waste residue behind the extraction macleaya cordata total alkaloid can also utilize as organic fertilizer or fuel again, can make the Herba Macleayae Cordatae resource be used fully and develop.
The specific embodiment
Embodiment 1
Infruit of Herba Macleayae Cordatae is crushed to the 40-60 order for 500 kilograms, join in the ultrasound wave counterflow extraction apparatus, add 2500 kilogram of 90% ethanol by the other end and carry out the adverse current supersound extraction, supersonic frequency is that 30-60KHz, ultrasonic time are 15-75 minute, ultrasonic power 12-76KW, extracting 50-80 ℃ of temperature, controlling solid-liquid ratio with fluid flowmeter and charging rate controller is 1: 5, and extracting solution separates slag liquid, extracting solution feeding liquid processing system through the slag liquid/gas separator; Adding 25 kilograms of 5ppmZTC 1+1 natural clarifying agent precipitations in settling tank goes part to remove albumen, tannin, macromolecular substances such as polysaccharide, add 30 kilograms of 5ppm kieselguhr and help filter, leaching Herba Macleayae Cordatae crude extract aqueous solution dope, coarse filtration (active carbon+quartz sand), three grades of doughnut membrane filtrations, remove mechanical admixture in the solution, enter micro-filtration membrane and carry out microfiltration, the reuse pure water is made into 1～2 ° of Be ' aqueous solution, carry out ultrafiltration purification, the operating pressure of ultrafiltration purification is 0.5-0.8MPa, adopting molecular cut off is 50000 ultrafiltration ceramic membrane filters, the material that further separates macromolecular substances and small-molecule substance, selecting molecular cut off then is that 500 NF membrane concentrate, concentrated solution gets 4.5 kilograms of macleaya cordata total alkaloids through Intelligentized static microwave vacuum drying, pulverizes with 100 order jet mills, and detecting macleaya cordata total alkaloid content with HPLC is 78.41%, extraction ratio is 0.9%, the packing warehouse-in.
Embodiment 2
Infruit of Herba Macleayae Cordatae is crushed to the 40-60 order for 500 kilograms, join in the ultrasound wave counterflow extraction apparatus, add pure water by the other end and carry out the adverse current supersound extraction, supersonic frequency is that 30-60KHz, ultrasonic time are 15-75 minute, ultrasonic power 12-76KW, extracting 50-80 ℃ of temperature, controlling solid-liquid ratio with fluid flowmeter and charging rate controller is 1: 5, and extracting solution separates slag liquid, extracting solution feeding liquid processing system through the slag liquid/gas separator; Adding 25 kilograms of 5ppmZTC 1+1 natural clarifying agent precipitations in settling tank goes part to remove albumen, tannin, macromolecular substances such as polysaccharide, add 30 kilograms of 5ppm kieselguhr and help filter, leaching Herba Macleayae Cordatae crude extract aqueous solution dope, coarse filtration (active carbon+quartz sand), three grades of doughnut membrane filtrations, remove mechanical admixture in the solution, enter micro-filtration membrane and carry out microfiltration, the reuse pure water is made into 1～2 ° of Be ' aqueous solution, carry out ultrafiltration purification, operating pressure is 0.5MPa, and adopting molecular cut off is 50000 ultrafiltration ceramic membrane filters, the material that further separates macromolecular substances and small-molecule substance, selecting molecular cut off then is that 500 NF membrane concentrate.Concentrated solution gets 3.5 kilograms of macleaya cordata total alkaloids through Intelligentized static microwave vacuum drying, pulverizes with 100 order jet mills, and be 64.61% with the HPLC detection level, extraction ratio is 0.7%, the packing warehouse-in.
Claims (8)
1. method for preparing macleaya cordata total alkaloid adopts that the ultrasound wave adverse current is extracted continuously, technology such as ceramic membrane purification, sodium filter membrane concentrate, Intelligentized static microwave vacuum drying technology, may further comprise the steps:
(1) the ultrasound wave adverse current is extracted continuously:
A, infruit of Herba Macleayae Cordatae is pulverized;
B, the infruit of Herba Macleayae Cordatae powder that will crush by solid-liquid ratio add in the continuous flow upstream ultrasonic device;
C, extracting solution is pumped into dosing pump at the equipment other end and to carry out the adverse current supersound extraction in the equipment;
D, extracting solution carry out slag liquid with dreg-liquid separator to be separated;
E, add 1-10% clarifier, filter aid in the extracting solution, remove precipitate through vacuum filtration, filtrate enters reclaims concentration systems and reclaims in the extracting solution organic solvent to not containing organic solvent, Herba Macleayae Cordatae crude extract aqueous solution dope;
(2), ceramic membrane separates
1.. get Herba Macleayae Cordatae crude extract aqueous solution coarse filtration, three grades of doughnut membrane filtrations are removed mechanical admixture in the solution, enter micro-filtration membrane and carry out microfiltration;
2.. the Herba Macleayae Cordatae crude extract (by volume) behind the microfiltration is made into the 1-5% diluent with pure water, use the ceramic super-filtering film ultrafiltration, further remove macromolecular substances such as albumen, pigment, polysaccharide and inorganic salt, micromolecule pigment, monosaccharide and the ash micromolecule thing impurity that grades;
(3) the sodium filter membrane concentrates
Herba Macleayae Cordatae essence extract liquid behind the ceramic membrane purification is concentrated into 5-20 ° of Be ' by the sodium filter membrane;
(4), Intelligentized static microwave vacuum drying
5-20 ° of Be ' concentrated solution used the drying machine drying at 20-50 ℃, and 〉=100 order jet mills are pulverized, and get product.
2. the method for preparing the Chinese medicine macleaya cordata total alkaloid according to claim 1, the grinding particle size scope that it is characterized in that described Herba Macleayae Cordatae are 40 orders-60 orders.
3. the method for preparing macleaya cordata total alkaloid according to claim 1 is characterized in that described extracting solution is that described solvent is to use pure water, also can be methanol, and ethanol, ethyl acetate are wherein a kind of.
4. the method for preparing macleaya cordata total alkaloid according to claim 1 is characterized in that described supersonic frequency is that 30-60KHz, ultrasonic time are the 15-75 branch, and ultrasonic power 12-76KW extracts 50-80 ℃ of temperature, and solid-liquid ratio is 1: 5.
5. the method for preparing macleaya cordata total alkaloid according to claim 1, it is characterized in that described clarifier is silicon dioxide gel (Silica sol), the higher derivative of chitosan, ZTC 1+1 natural clarifying agent, carrageenan, Bentonite (Bentonite), crospovidone (PVPP); Filter aid is a kieselguhr, silica flour, and perlite also can be a Pulvis Talci.
6. the method for preparing macleaya cordata total alkaloid according to claim 1 is characterized in that described ceramic super-filtering film, adopts molecular cut off to purify for the 10000-30000 ceramic membrane.
7. the method for preparing macleaya cordata total alkaloid according to claim 1 is characterized in that described sodium filter membrane concentrates, and adopts 500-1000 sodium filter membrane to concentrate.
8. the method for preparing macleaya cordata total alkaloid according to claim 1 is characterized in that described drying machine is vacuum microwave drier, round vacuum microwave drier, square vacuum microwave drier or drying machine with centrifugal spray.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103769608A (en) * | 2014-02-20 | 2014-05-07 | 北京碧水源膜科技有限公司 | Nano-silver sol separating method |
| CN104825510A (en) * | 2015-04-28 | 2015-08-12 | 厦门理工学院 | Membrane method for extracting total alkaloids from rauvolfia verticillata |
| CN109331974A (en) * | 2018-10-12 | 2019-02-15 | 湖南美可达生物资源股份有限公司 | A kind of macleaya cordata ultrasound micro mist crushing device and macleaya cordata total alkaloid ultrasound assisted extraction technique |
| CN109369729A (en) * | 2018-09-06 | 2019-02-22 | 铜仁职业技术学院 | A kind of method that inner ebullition method extracts Macleaya cordata alkaloids |
| CN110961231A (en) * | 2019-12-23 | 2020-04-07 | 金晓飞 | Preparation method and application of macleaya cordata traditional Chinese medicinal material ultramicro wall-breaking powder |
Citations (1)
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| CN101020703A (en) * | 2006-11-01 | 2007-08-22 | 郁建生 | Total alkaloid of pink plumepoppy herb |
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| CN101020703A (en) * | 2006-11-01 | 2007-08-22 | 郁建生 | Total alkaloid of pink plumepoppy herb |
Non-Patent Citations (2)
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| 范家佑 ,郁建平 ,胡美忠，等: "博落回生物碱酸水提取工艺及优化", 《安徽农业科学》, vol. 38, no. 19, 31 October 2010 (2010-10-31) * |
| 马爱瑛: "生物碱的提取与分离", 《固原师专学报(自然科学)》, no. 3, 31 May 2006 (2006-05-31), pages 25 - 30 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103769608A (en) * | 2014-02-20 | 2014-05-07 | 北京碧水源膜科技有限公司 | Nano-silver sol separating method |
| CN104825510A (en) * | 2015-04-28 | 2015-08-12 | 厦门理工学院 | Membrane method for extracting total alkaloids from rauvolfia verticillata |
| CN109369729A (en) * | 2018-09-06 | 2019-02-22 | 铜仁职业技术学院 | A kind of method that inner ebullition method extracts Macleaya cordata alkaloids |
| CN109331974A (en) * | 2018-10-12 | 2019-02-15 | 湖南美可达生物资源股份有限公司 | A kind of macleaya cordata ultrasound micro mist crushing device and macleaya cordata total alkaloid ultrasound assisted extraction technique |
| CN109331974B (en) * | 2018-10-12 | 2019-07-02 | 湖南美可达生物资源股份有限公司 | A kind of macleaya cordata ultrasound micro mist crushing device and ultrasound assisted extraction technique |
| CN110961231A (en) * | 2019-12-23 | 2020-04-07 | 金晓飞 | Preparation method and application of macleaya cordata traditional Chinese medicinal material ultramicro wall-breaking powder |
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