CN104958336A - Method for purifying panax notoginseng saponins by combining ultrafiltration and nanofiltration technologies - Google Patents
Method for purifying panax notoginseng saponins by combining ultrafiltration and nanofiltration technologies Download PDFInfo
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- CN104958336A CN104958336A CN201510396277.5A CN201510396277A CN104958336A CN 104958336 A CN104958336 A CN 104958336A CN 201510396277 A CN201510396277 A CN 201510396277A CN 104958336 A CN104958336 A CN 104958336A
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Abstract
The invention discloses a method for purifying panax notoginseng saponins by combining ultrafiltration and nanofiltration technologies. The method comprises the following processes of panax notoginseng preparation, smashing, ethanol extraction, macroporous resin column feeding, aluminum column peroxidation, titanium rod filtration, ultrafiltration, nanofiltration, concentration, drying, smashing again and panax notoginseng saponins obtaining, wherein the operation conditions of the ultrafiltration and nanofiltration working procedures are as follows: the liquid feeding pressure is 0.15-0.4Mpa, the material liquid flowing speed is 20-30ml/s, and the material liquid temperature is 20-30 DEG C; ultrafiltration is repeatedly carried out for multiple times; the pH value of the material liquid is controlled at 6.2-7.4; during backwashing, the backwashing is carried out in each batch, and the backwashing time is 1.2h; the rejection molecular weight of an ultrafiltration membrane of the ultrafiltration working procedure is 20,000-90,000Da; the rejection molecular weight of a nanofiltration membrane of the nanofiltration working procedure is 600-800Da; by application of the ultrafiltration and nanofiltration technologies in a production production for extracting panax notoginseng saponins from panax notoginseng, the panax notoginseng saponins is further purified.
Description
Technical field
The present invention relates to and relate to biological pharmacy technical field, specifically, is the Radix Notoginseng total arasaponins method of purification that a kind of ultrafiltration and nanofiltration combine.
Background technology
Radix Notoginseng total arasaponins (Radix Notoginseng total arasaponins), cures mainly blood circulation promoting and blood stasis dispelling, promotes blood circulation active.There is the effect of anticoagulant and increase cerebral blood flow, for cerebrovascular sequelae, central retinal vein occlusion, hyphema etc.
Modern pharmacology research shows, Radix Notoginseng total arasaponins is the principle active component of Radix Notoginseng.Radix Notoginseng total arasaponins has following pharmacology, efficacy effect:
Effect to hyperlipemia:
With Radix Notoginseng total arasaponins, hyperlipidemia patient is carried out to the clinical research of blood fat reducing antithrombotic effect.Have obvious antiplatelet aggregation after result treatment and fall fine effect, the improvement of clinical efficacy and blood fat, hemorheology is all better than matched group.Research shows that Radix Notoginseng total arasaponins has obvious preventive and therapeutic action to hyperlipemia.
Effect to high blood viscosity:
High blood viscosity patient is divided into Radix Notoginseng total arasaponins group and enteric coated aspirin group, through 4 weeks 1 course of therapy, result shows that Radix Notoginseng total arasaponins has and significantly reduces surface activity of blood platelet, suppresses platelet adhesion and gathering, antithrombus formation, improves the effects such as microcirculation, and be better than aspirin.
To hypertensive effect:
Treat hypertension with Radix Notoginseng total arasaponins, treat after 20 days, obviously can reduce the blood pressure that increases can also obvious decreased heart rate, result display Radix Notoginseng total arasaponins can significantly reduce hyperpietic MDA, obvious increased SOD, increases erythrocyte deformability, reduces erythrocytic aggregation.
Function of resisting myocardial ischemia:
With Radix Notoginseng total arasaponins, expeirmental myocardial ischemia Functional observation is found that Radix Notoginseng total arasaponins significantly can improve the ischemia performance of surface electrocardiogram, reduce myocardial infarct size, the Left ventricular dilatation dysfunction of reversible angina of effort patient, even can make it to recover normal.
Arrhythmia:
With the Functional observation of Radix Notoginseng total arasaponins On Antagonizing Experimental Arrhythmia, zoopery display Radix Notoginseng total arasaponins can make rat experimental ventricular premature contraction obviously reduce, the arrhythmia persistent period obviously shortens, ARR incidence rate during Reperfu-sion after the acute myocardial infarction of obvious reduction rat.
Study of anti-atherogenic effect:
Observe Radix Notoginseng total arasaponins to the atherosclerotic impact of rabbit bait; show that Radix Notoginseng total arasaponins can by antiinflammatory and antioxidative effect; play the effect of anti-AS; protective effect is had to vascular smooth muscle cell; energy Cell protection, by the impact of Hyperlipidemic Serum, has certain preventive and therapeutic effect to atherosclerotic generation and development.
Antithrombus formation, improving micro_circulation effect:
Research Radix Notoginseng total arasaponins is on the impact of patients with coronary artery disease ET-1 and platelet function, and result display Radix Notoginseng total arasaponins has and significantly reduces surface activity of blood platelet, anticoagulant and sticking, and antithrombus formation, improves the effects such as microcirculation.
Anti-cardiac-cerebral ischemia effect:
Adopt Radix Notoginseng total arasaponins treatment cerebral infarction and ischemic cerebrovascular, result shows that Radix Notoginseng total arasaponins has good clinical therapeutic efficacy to Acute Cerebral Infarction, and Radix Notoginseng total arasaponins significantly can improve the cerebral edema during global brain ischemia or focal cerebral ischemia-reperfusion injury.
Promote hematopoietic growth:
Radix Notoginseng total arasaponins has proliferation function to hemopoietic progenitor cell, research also finds that Rg1 and Rb1 in Radix Notoginseng total arasaponins is the effective monomer promoting hemopoietic, constantly can promote the propagation of people's bone marrow granulocyte, hemopoietic progenitor cell of red blood cell line, CFU-E is better than to the effect of grain system CFU-GM.
Fibrosis:
Find that Radix Notoginseng total arasaponins can delay renal tubules from cellular level research---interstitial fibrosis process, improve renal function.Experiment finds that Radix Notoginseng total arasaponins can make alveolitis time of origin postpone, and makes slow progress, and degree is comparatively light, forms lung fiber hardly.
By the effect of animal experiment study Radix Notoginseng total arasaponins to Experimental Liver Fibrosis, result display arasaponin has obvious effect of anti hepatic fibrosis.
Protective effect to neural cell injury:
By cytology, the protective effect of Radix Notoginseng total arasaponins to model cell is observed in the detection of morphology and lipid peroxidation injury index, and result shows that Radix Notoginseng total arasaponins has protective effect to the neural cell injury that energy metabolism impairment causes.
Membrance separation occurs in 20 beginnings of the century, the separation technology emerged rapidly after the sixties in 20th century.Membrane separation technique is owing to having separation, concentrated, purification and refining function concurrently, there are again efficient, energy-saving and environmental protection, molecule level is filtered and filter process is simple, be easy to the features such as control, therefore, food, medicine, biology, environmental protection, chemical industry, metallurgy, the energy, oil, water treatment, electronics, the field such as bionical are widely used at present, create huge economic benefit and social benefit, become one of most important means in current separation science.
Ultrafiltration is a kind of membrane separation technique, its main part is ultrafilter membrane, for the separation of material macromole rank in solution, ultra-filtration process is for power with film pressure at both sides difference, a kind of solution separating process based on mechanical grading principle, use pressure to be generally 0.1Mpa-0.25Mpa, be separated 1 μm-0.1 μm, aperture molecular cut off about 500-1000000Dalton.Ultrafiltration is different from all conventional filtrations and microporous filter (being static filtering), and one is that ultra-filtration and separation footpath is little, almost can retain all antibacterials, virus and colloidal particles in solution, protein, larger molecular organics.Two is that whole filter process carries out in a dynamic state, and solvent only obtains the separation of part.Enter the material liquid of ultrafiltration module, under the promotion of film pressure at both sides difference, component permeate film becomes ultrafiltrate, and all the other then become concentrated solution and continuously outflow, and makes film surface can not be only limited gathering through material.Filtering rate can reach an equilibrium valve and unlikely continuous decay at steady state, and whole process can continue for a long time.
Nanofiltration is also a kind of membrane separation technique, optional from 200 ~ 1000Dalton to rejection to organics molecular weight, has moderate above removal efficiency to salt.There is inspissation simultaneously.
Ultrafiltration, Nanofiltration Membrane Separation Technology are comparatively suitable for the particular/special requirement of some process procedures realized in existing extraction of traditional Chinese medicine, are conducive to the inherence and the external quality that improve Chinese medicine compound preparation.
Current is raw material with Radix Notoginseng, extracts the production technology of Radix Notoginseng total arasaponins, the small-molecule substance impurity such as inorganic salt and part macromolecular substances impurity can't be eliminated, make XUESAITONG, XUESHUANTONG ZHUSHEYE existence and stability, safety issue.
Summary of the invention
The object of the present invention is to provide the Radix Notoginseng total arasaponins method of purification that a kind of ultrafiltration and nanofiltration combine, the application in Radix Notoginseng total arasaponins production technology is extracted Radix Notoginseng by ultrafiltration and nanofiltration, further purification Radix Notoginseng total arasaponins, retain the low molecule such as macromolecule and inorganic salt impurity, meet the needs of pin raw material.Also can be used for taking Radix Notoginseng total arasaponins as raw material, the preparation production technique of preparation XUESAITONG ZHUSHEYE.
The present invention is achieved through the following technical solutions: the Radix Notoginseng total arasaponins method of purification that a kind of ultrafiltration and nanofiltration combine, comprises following technique: Radix Notoginseng → pulverizing → alcohol steep → upper macroporous resin column → peroxidating aluminum post → titanium rod filtration → ultrafiltration → nanofiltration → concentrated → drying → pulverizing → Radix Notoginseng total arasaponins; Wherein, the operating condition of ultrafiltration, nanofiltration operation is as follows:
1) inlet hydraulic is 0.15 ~ 0.4Mpa;
2) feed velocity is 20 ~ 30ml/s;
3) feed temperature is 20 ~ 30 DEG C;
4) when feed liquid stock solution is extremely a small amount of by ultrafiltration, then add purified water dilution, repeat ultrafiltration repeatedly;
5) pH value of feed liquid controls 6.2 ~ 7.4;
6) backwash: backwashing period is for often to criticize, and backwashing time is 1.2h;
The molecular cut off of the ultrafilter membrane of described ultrafiltration operation adopts 20000 ~ 90000Da, and the molecular cut off of the NF membrane of described nanofiltration operation adopts 600 ~ 800Da.
To better implement the present invention, further, the ultrafiltration membrane material of described ultrafiltration operation adopts polysulfones membrane material, polypropylene, composite polrvinyl chloride; The NF membrane material of described nanofiltration operation adopts aromatic polyamide composite membrane.
Further, to better implement the present invention, in described ultrafiltration operation, ultrafilter membrane membrane structure adopts hollow fiber ultrafiltration membrane, rolling or tubular ultra-filtration membrane, adopts cross flow filter or adopt dead-end filtration when ultrafiltration.
Compared with prior art, the present invention has following beneficial effect:
The present invention extracts the application in Radix Notoginseng total arasaponins production technology by ultrafiltration and nanofiltration Radix Notoginseng, and Radix Notoginseng total arasaponins of purifying further, retains the low molecule such as macromolecule and inorganic salt impurity, meet the needs of pin raw material.Also can be used for taking Radix Notoginseng total arasaponins as raw material, the preparation production technique of preparation XUESAITONG ZHUSHEYE.
The present invention's ultrafiltration is separated Radix Notoginseng total arasaponins with nanofiltration, concentrate, refining, having the advantages such as production procedure is simple, easy and simple to handle, good separating effect, bioactive substance are destroyed, is very desirable impurity-removing method.Can effectively remove the small-molecule substance impurity such as macromolecular substances impurity and inorganic salt, the purity of Radix Notoginseng total arasaponins can be improved.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, and embodiments of the present invention include but not limited to the following example.
Embodiment 1:
The Radix Notoginseng total arasaponins method of purification that ultrafiltration and nanofiltration combine, comprises following technique: Radix Notoginseng → pulverizing → alcohol steep → upper macroporous resin column → peroxidating aluminum post → titanium rod filtration → ultrafiltration → nanofiltration → concentrated → drying → pulverizing → Radix Notoginseng total arasaponins; Wherein, the operating condition of ultrafiltration, nanofiltration operation is as follows:
1) inlet hydraulic is 0.15 ~ 0.4Mpa;
2) feed velocity is 20 ~ 30ml/s;
3) feed temperature is 20 ~ 30 DEG C;
4) when feed liquid stock solution is extremely a small amount of by ultrafiltration, then add purified water dilution, repeat ultrafiltration repeatedly;
5) pH value of feed liquid controls 6.2 ~ 7.4;
6) backwash: backwashing period is for often to criticize, and backwashing time is 1.2h;
The molecular cut off of the ultrafilter membrane of described ultrafiltration operation adopts 20000 ~ 90000Da, and the molecular cut off of the NF membrane of described nanofiltration operation adopts 600 ~ 800Da.
Embodiment 2:
The present embodiment is at the enterprising one-step optimization in the basis of above-described embodiment, and to better implement the present invention, further, the ultrafiltration membrane material of described ultrafiltration operation adopts polysulfones membrane material, polypropylene, composite polrvinyl chloride; The NF membrane material of described nanofiltration operation adopts aromatic polyamide composite membrane.
Embodiment 3:
The present embodiment is at the enterprising one-step optimization in the basis of above-mentioned any embodiment, further, to better implement the present invention, in described ultrafiltration operation, ultrafilter membrane membrane structure adopts hollow fiber ultrafiltration membrane, rolling or tubular ultra-filtration membrane, adopts cross flow filter or adopt dead-end filtration when ultrafiltration.
Embodiment 4:
The present embodiment is at the enterprising one-step optimization in the basis of above-described embodiment, the Radix Notoginseng total arasaponins method of purification that a kind of ultrafiltration and nanofiltration combine:
Raw material: Radix Notoginseng
Membrane material: ultrafiltration membrane material is composite polrvinyl chloride, molecular cut off is 20000Da, and version is hollow fiber ultrafiltration membrane; NF membrane material aromatic polyamide composite membrane, molecular cut off is 600Da.
Radix Notoginseng → pulverizing → alcohol steep → upper macroporous resin column → peroxidating aluminum post → add appropriate needle-use activated carbon, titanium rod filtration → ultrafiltration → nanofiltration → concentrated → drying → pulverizing → Radix Notoginseng total arasaponins.Wherein, Radix Notoginseng → pulverizing → alcohol steep → upper macroporous resin column → peroxidating aluminum post → add appropriate needle-use activated carbon, the process that titanium rod filters, and the process of concentrated → drying → pulverizing → Radix Notoginseng total arasaponins is all undertaken by existing method.
Ultrafiltration adopts dead-end filtration, and the inlet-pressure of ultrafiltrate is 0.15MPa, and liquid outlet pressure ratio inlet pressure is low, and feed velocity is 21.12mL/s; Feed temperature is 22 DEG C; The pH value 6.8 of feed liquid; When feed liquid stock solution by ultrafiltration to time a small amount of, then adding purified water, to be diluted to proportion be 1.05 continuation ultrafiltration, repeats ultrafiltration repeatedly; After technical process terminates, to titanium rod filtrate, liquid and the concentrated Radix Notoginseng total arasaponins highly finished product liquid formed compare more than ultrafiltration:
Also can be used for taking Radix Notoginseng total arasaponins as raw material, the preparation production technique of preparation XUESAITONG ZHUSHEYE.Namely Radix Notoginseng total arasaponins adds water for injection, and active carbon is boiled → adds in mixing, filter and fine straining → ultrafiltration → nanofiltration → add sodium chloride appropriate, adjust ph water dilutes in right amount, obtains XUESAITONG ZHUSHEYE.
Embodiment 5:
The present embodiment is at the enterprising one-step optimization in the basis of above-described embodiment, the Radix Notoginseng total arasaponins method of purification that a kind of ultrafiltration and nanofiltration combine:
Raw material: Radix Notoginseng
Membrane material: ultrafiltration membrane material is polypropylene, molecular cut off is 50000, and version is hollow fiber ultrafiltration membrane; NF membrane material aromatic polyamide composite membrane, molecular cut off is 700.
Radix Notoginseng → pulverizing → alcohol steep → upper macroporous resin column → peroxidating aluminum post → add appropriate needle-use activated carbon, titanium rod filtration → ultrafiltration → nanofiltration → concentrated → drying → pulverizing → Radix Notoginseng total arasaponins.Wherein, Radix Notoginseng → pulverizing → alcohol steep → upper macroporous resin column → peroxidating aluminum post → add appropriate needle-use activated carbon, the process that titanium rod filters, and the process of concentrated → drying → pulverizing → Radix Notoginseng total arasaponins is all undertaken by existing method.
Ultrafiltration adopts cross flow filter, and the inlet-pressure of ultrafiltrate is 0.25MPa, and liquid outlet pressure ratio inlet pressure is low, and feed velocity is 25.25mL/s; Feed temperature is 25 DEG C; The pH value 7.0 of feed liquid; When feed liquid stock solution by ultrafiltration to time a small amount of, then adding purified water, to be diluted to proportion be 1.15 continuation ultrafiltration, repeats ultrafiltration repeatedly; After technical process terminates, to titanium rod filtrate, liquid and the concentrated Radix Notoginseng total arasaponins highly finished product liquid formed compare more than ultrafiltration:
Also can be used for taking Radix Notoginseng total arasaponins as raw material, the preparation production technique of preparation XUESAITONG ZHUSHEYE.Namely Radix Notoginseng total arasaponins adds water for injection, and active carbon is boiled → adds in mixing, filter and fine straining → ultrafiltration → nanofiltration → add sodium chloride appropriate, adjust ph water dilutes in right amount, obtains XUESAITONG ZHUSHEYE.
Embodiment 6:
The present embodiment is at the enterprising one-step optimization in the basis of above-described embodiment, the Radix Notoginseng total arasaponins method of purification that a kind of ultrafiltration and nanofiltration combine:
Raw material: Radix Notoginseng
Membrane material: ultrafiltration membrane material is polysulfones membrane material, molecular cut off is 90000, and version is hollow fiber ultrafiltration membrane; NF membrane material aromatic polyamide composite membrane, molecular cut off is 800.
Radix Notoginseng → pulverizing → alcohol steep → upper macroporous resin column → peroxidating aluminum post → add appropriate needle-use activated carbon, titanium rod filtration → ultrafiltration → nanofiltration → concentrated → drying → pulverizing → Radix Notoginseng total arasaponins.Wherein, Radix Notoginseng → pulverizing → alcohol steep → upper macroporous resin column → peroxidating aluminum post → add appropriate needle-use activated carbon, the process that titanium rod filters, and the process of concentrated → drying → pulverizing → Radix Notoginseng total arasaponins is all undertaken by existing method.
Ultrafiltration adopts cross flow filter, and the inlet-pressure of ultrafiltrate is 0.4MPa, and liquid outlet pressure ratio inlet pressure is low, and feed velocity is 28.12mL/s; Feed temperature is 28 DEG C; The pH value 7.4 of feed liquid; When feed liquid stock solution by ultrafiltration to time a small amount of, then adding purified water, to be diluted to proportion be 1.2 continuation ultrafiltration, repeats ultrafiltration repeatedly; After technical process terminates, to titanium rod filtrate, liquid and the concentrated Radix Notoginseng total arasaponins highly finished product liquid formed compare more than ultrafiltration:
Also can be used for taking Radix Notoginseng total arasaponins as raw material, the preparation production technique of preparation XUESAITONG ZHUSHEYE.Namely Radix Notoginseng total arasaponins adds water for injection, and active carbon is boiled → adds in mixing, filter and fine straining → ultrafiltration → nanofiltration → add sodium chloride appropriate, adjust ph water dilutes in right amount, obtains XUESAITONG ZHUSHEYE.
The above is only preferred embodiment of the present invention, and not do any pro forma restriction to the present invention, every any simple modification, equivalent variations done above embodiment according to technical spirit of the present invention, all falls within protection scope of the present invention.
Claims (3)
1. the Radix Notoginseng total arasaponins method of purification that combines of ultrafiltration and nanofiltration, is characterized in that: comprise following technique: Radix Notoginseng → pulverizing → alcohol steep → upper macroporous resin column → peroxidating aluminum post → titanium rod filtrations → ultrafiltration → nanofiltration → concentrate → drying → pulverizing → Radix Notoginseng total arasaponins; Wherein, the operating condition of ultrafiltration, nanofiltration operation is as follows:
1) inlet hydraulic is 0.15 ~ 0.4Mpa;
2) feed velocity is 20 ~ 30ml/s;
3) feed temperature is 20 ~ 30 DEG C;
4) when feed liquid stock solution is extremely a small amount of by ultrafiltration, then add purified water dilution, repeat ultrafiltration repeatedly;
5) pH value of feed liquid controls 6.2 ~ 7.4;
6) backwash: backwashing period is for often to criticize, and backwashing time is 1.2h;
The molecular cut off of the ultrafilter membrane of described ultrafiltration operation adopts 20000 ~ 90000Da, and the molecular cut off of the NF membrane of described nanofiltration operation adopts 600 ~ 800Da.
2. the Radix Notoginseng total arasaponins method of purification that combines of a kind of ultrafiltration according to claim 1 and nanofiltration, is characterized in that: the ultrafiltration membrane material of described ultrafiltration operation adopts polysulfones membrane material, polypropylene, composite polrvinyl chloride; The NF membrane material of described nanofiltration operation adopts aromatic polyamide composite membrane.
3. the Radix Notoginseng total arasaponins method of purification that combines of a kind of ultrafiltration according to claim 1 and 2 and nanofiltration, it is characterized in that: in described ultrafiltration operation, ultrafilter membrane membrane structure adopts hollow fiber ultrafiltration membrane, rolling or tubular ultra-filtration membrane, adopts cross flow filter or adopt dead-end filtration when ultrafiltration.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1751676A (en) * | 2004-09-22 | 2006-03-29 | 天津天士力制药股份有限公司 | Diaphragm ultrafiltration method for refining traditional Chinese medicine |
| CN101450091B (en) * | 2008-12-30 | 2012-06-27 | 云南云科药业有限公司 | Purification method of Panax notoginseng saponins |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1751676A (en) * | 2004-09-22 | 2006-03-29 | 天津天士力制药股份有限公司 | Diaphragm ultrafiltration method for refining traditional Chinese medicine |
| CN101450091B (en) * | 2008-12-30 | 2012-06-27 | 云南云科药业有限公司 | Purification method of Panax notoginseng saponins |
Non-Patent Citations (1)
| Title |
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| 潘艺 等: "中草药有效成分分离技术研究进展", 《广东农业科学》 * |
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Application publication date: 20151007 |