CN101450091B - Purification method of Panax notoginseng saponins - Google Patents
Purification method of Panax notoginseng saponins Download PDFInfo
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- CN101450091B CN101450091B CN2008102337758A CN200810233775A CN101450091B CN 101450091 B CN101450091 B CN 101450091B CN 2008102337758 A CN2008102337758 A CN 2008102337758A CN 200810233775 A CN200810233775 A CN 200810233775A CN 101450091 B CN101450091 B CN 101450091B
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Abstract
The invention relates to a notoginsen triterpenes purifying method using ultra-filtration and nano-filtration technology to extract trashes and purify the notoginsen triterpenes in notoginsen triterpenes production process using notoginseng as raw material. That is: notoginseng-> smashing-> enthanol eluting-> passing macroporous resin column-> passing alumina column->adding an amount of needle used active carbon, titanium rod filtering-> ultra-filtering-> nano-filtering-> refining and concentrating->drying->smashing-> notoginsen triterpenes. The process can also be used in Xuesaitong injection production process using notoginsen triterpenes as raw material. That is: adding water for injection into notoginsen triterpenes, mixing and boiling-> adding active carbon, filtering and fine-filtering->ultra-filtering->nano-filtering->adding an amount of sodium chloride, regulating pH value, diluting by an amount of water and obtaining the Xuesaitong injection. The invention achieves the advantages of simple production process, simple operation, good separation effect and no damage to bioactive substances, can eliminate macromolecular substance impurity and micromolecule substance impurity such as inorganic salt, thereby improving the purity of notoginsen triterpenes.
Description
Technical field
The present invention relates to a kind of method with ultrafiltration and nanofiltration purification Radix Notoginseng total arasaponins.
Background technology
Membrance separation is to occur in 20 beginnings of the century, a separation technology that emerges rapidly after the sixties in 20th century.Membrane separation technique is owing to have separations, concentrated, purification and purified function concurrently; Efficient, energy-saving and environmental protection are arranged again, molecular level filters and filter process is simple, be easy to characteristic such as control; Therefore; Be widely used in food, medicine, biology, environmental protection, chemical industry, metallurgy, the energy, oil, water treatment, electronics, field such as bionical at present, produced huge economic benefit and social benefit, become one of most important means in the current separation science.
Ultrafiltration is a kind of membrane separation technique; Its main part is a ultrafilter membrane, is used for other separation of solution material macromole level, and ultra-filtration process is to be power with film pressure at both sides difference; A kind of solution separating process that is the basis with the mechanical grading principle; Working pressure is generally 0.1Mpa-0, and 25Mpa separates about the 1 μ m-0.1 μ m molecular cut off 500-1000000Dalton of aperture.Ultrafiltration is different with all conventional filtrations and microporous filter (being static filtering), and the one, the ultra-filtration and separation footpath is little, almost can hold back all antibacterials, virus and colloidal particles in the solution, protein, larger molecular organics.The 2nd, whole filter process carries out under dynamically, and solvent only obtains the separation of part.Get into the material liquid of ultrafiltration module, under the promotion of film pressure at both sides difference, part sees through film becomes ultrafiltrate, and all the other then become concentrated solution and pour, and make the film surface can not see through material and be merely limited gathering.Filtering rate can reach an equilibrium valve and unlikely continuous decay under steady statue, whole process can continue for a long time.
Nanofiltration also is a kind of membrane separation technique, and is optional from 200～1000Dalton to the rejection to organics molecular weight, and salt is had moderate above removal efficiency.Has inspissation simultaneously.
Ultrafiltration, nanofiltration membrane separation technology are suitable for realizing the specific (special) requirements of some process procedures in the existing Chinese medicine extraction process, help improving the inherence and the external quality of Chinese medicine compound preparation.
Along with rapid development of national economy, the application of membrane separation technique not only can be more and more widely, and it can and be accepted by increasing people's understanding.According to the preliminary statistics; Calendar year 2001 whole world film and the sales volume of membrane module near 8,000,000,000 US dollars; The market of complete set of equipments and film engineering has then reached tens billion of US dollars, and also increases progressively in the amplitude with 10%～20% every year, demonstrates the bright prospects of this new industry.
The quality problems of Chinese medicine cause concern day by day in recent years; And XUESAITONG, XUESHUANTONG ZHUSHEYE that preparation consists of the Radix Notoginseng total arasaponins sodium chloride injection also exist medicine stability, safety issue as one of maximum Chinese medicine kind of sales volume in the market.Its main cause is because the complex chemical composition of Chinese medicine own has materials such as protein, vitamin, organic acid, saccharide, aminoacid, oils and fats, wax, enzyme, pigment, tannin, inorganic salt, volatile oil, alkaloid, glycoside usually.Wherein existing effective ingredient has invalid impurity again, just owing to impurity such as inorganic salt, tannin, protein and macromolecular substances are not effectively removed, has just influenced stability of formulation and safety.Be raw material at present with the Radix Notoginseng, extract the production technology of Radix Notoginseng total arasaponins, can't small-molecule substance impurity such as inorganic salt and part macromolecular substances impurity be eliminated, make XUESAITONG, XUESHUANTONG ZHUSHEYE have stability, safety issue.
Summary of the invention
The objective of the invention is to extract the application in the Radix Notoginseng total arasaponins production technology through membrane ultrafiltration and nanofiltration Radix Notoginseng, the Radix Notoginseng total arasaponins of further purifying is held back low molecular impurities such as macromolecule and inorganic salt, satisfies the needs of pin with raw material.Also can be used for the Radix Notoginseng total arasaponins is raw material, the preparation production technique of preparation XUESAITONG ZHUSHEYE.
The present invention increases membrane ultrafiltration, nanofiltration in existing Radix Notoginseng total arasaponins production technology.Membrane ultrafiltration, nanofiltration technique are increased in after the titanium rod fillter section, and then concentrate.That is: an amount of needle-use activated carbon of Radix Notoginseng → pulverizing → ethanol lixiviate → go up macroporous resin column → peroxidating aluminum post → add, titanium rod filtrations → ultrafiltration → nanofiltration → refining is concentrated → drying → pulverizing → Radix Notoginseng total arasaponins.
Ultra-filtration process is held back macromolecule impurity; Nanofiltration process is held back small-molecular weight inorganic salt impurity, can concentrate filtrating simultaneously, realizes that purification concentrates purpose.
The molecular cut off of above-mentioned ultrafilter membrane generally is adopted as 10000～100000Da, preferred 100000Da.The molecular cut off of NF membrane adopts 200～500Da.
Membrane structure of the present invention can adopt hollow fiber ultrafiltration membrane, rolling or tubular ultra-filtration membrane, preferred rolling ultrafilter membrane.Both can adopt cross flow filter, also can adopt dead-end filtration, preferred cross flow filter.
The operating condition of ultrafiltration, nanofiltration technique is following:
1) inlet hydraulic is 0.1～0.5Mpa;
2) the feed liquid flow velocity is 0～55ml/s, preferred 10～40ml/s;
3) feed temperature is 15～50 ℃, is preferably 20～40 ℃;
4) when feed liquid stock solution is extremely a small amount of by ultrafiltration, add the purified water dilution again, repeat ultrafiltration repeatedly;
5) pH value of feed liquid is controlled at 5～9, and preferred 6.0～7.5;
6) backwash: backwashing period is every batch, and backwashing time is 1.5h;
The present invention also is applicable to the Radix Notoginseng total arasaponins to be raw material simultaneously, produces the production process of injection.
The present invention with ultrafiltration and nanofiltration to Radix Notoginseng total arasaponins separate, concentrate, refining, advantage such as have that production procedure is simple, easy and simple to handle, good separating effect, bioactive substance are not destroyed is very ideal impurity-removing method.Small-molecule substance impurity such as macromolecular substances impurity and inorganic salt can be effectively removed, the purity of Radix Notoginseng total arasaponins can be improved.
The specific embodiment
Embodiment 1:
Raw material: Radix Notoginseng
Membrane material: the ultrafilter membrane material is a polypropylene, and molecular cut off is 10000, and version is hollow fiber ultrafiltration membrane; NF membrane material aromatic polyamide composite membrane, molecular cut off are 500.
An amount of needle-use activated carbon of Radix Notoginseng → pulverizing → ethanol lixiviate → go up macroporous resin column → peroxidating aluminum post → add, titanium rod filtrations → ultrafiltration → nanofiltration → refining is concentrated → drying → pulverizing → Radix Notoginseng total arasaponins highly finished product.Wherein, Radix Notoginseng → pulverizing → ethanol lixiviate → last macroporous resin column → peroxidating aluminum post → add an amount of needle-use activated carbon, the filtering process of titanium rod, and the process of refining concentrating → drying → pulverizing → Radix Notoginseng total arasaponins highly finished product is all undertaken by existing method.(below identical)
Cross flow filter is adopted in ultrafiltration, and the import of ultrafiltrate is pressed and is 0.1MPa, and liquid outlet pressure ratio inlet pressure is low, and the feed liquid flow velocity is 18.12mL/s; Feed temperature is 25 ℃; The pH value 6.45 of feed liquid; When feed liquid stock solution by ultrafiltration when a small amount of, adding purified water again, to be diluted to proportion be 1.03 to continue ultrafiltration, repeats ultrafiltration repeatedly; After technical process finishes, titanium rod filtrate, the surplus liquid of ultrafiltration and Radix Notoginseng total arasaponins highly finished product liquid are compared:
| Each constituent content | Titanium rod filtrate | The surplus liquid of ultrafiltration | The Radix Notoginseng total arasaponins highly finished product |
| R1 | 7.2 | 5.1 | 7.6 |
| Rg1 | 34.5 | 25.2 | 38.0 |
| Rb1 | 35.8 | 44.2 | 33.2 |
| Visible foreign matters | A small amount of point-like thing is arranged, and opalescence is shallow | The point-like thing is many, and opalescence is strong | Limpid, the point-like thing is few, no opalescence |
| pH | 6.45 | 6.49 | 6.70 |
| Color number | No. 4 | No. 5 | No. 2 |
Also can be used for the Radix Notoginseng total arasaponins is raw material, the preparation production technique of preparation XUESAITONG ZHUSHEYE.Be that Radix Notoginseng total arasaponins adds water for injection, mix and boil → add active carbon that filtration and fine straining → ultrafiltration → nanofiltration → adding sodium chloride are an amount of, regulate the pH value water and dilute in right amount, obtain XUESAITONG ZHUSHEYE.
Embodiment 2:
Raw material: Radix Notoginseng
Membrane material: the ultrafilter membrane material is a PS membrane, and molecular cut off is 100000, and version is hollow fiber ultrafiltration membrane; NF membrane material polyacrylonitrile, molecular cut off are 500.
An amount of needle-use activated carbon of Radix Notoginseng → pulverizing → ethanol lixiviate → go up macroporous resin column → peroxidating aluminum post → add, titanium rod filtrations → ultrafiltration → nanofiltration → refining is concentrated → drying → pulverizing → Radix Notoginseng total arasaponins highly finished product.
Cross flow filter is adopted in ultrafiltration, and the import of ultrafiltrate is pressed and is 0.15MPa, and liquid outlet pressure ratio inlet pressure is low, and the feed liquid flow velocity is 27.91mL/s.Feed temperature is 25 ℃; The pH value 7.24 of feed liquid; When feed liquid stock solution by ultrafiltration when a small amount of, adding purified water again, to be diluted to proportion be 1.03 to continue ultrafiltration, repeats ultrafiltration repeatedly; After technical process finishes, titanium rod filtrate, the surplus liquid of ultrafiltration and Radix Notoginseng total arasaponins highly finished product are compared:
| Each constituent content | Titanium rod filtrate | The surplus liquid of ultrafiltration | The Radix Notoginseng total arasaponins highly finished product |
| R1 | 6.2 | 5.1 | 6.1 |
| Rg1 | 32.5 | 27.0 | 32.0 |
| Rb1 | 37.0 | 42.0 | 35.3 |
| Visible foreign matters | A small amount of point-like thing is arranged, and opalescence is shallow | The point-like thing is many, and opalescence is strong | Limpid, the point-like thing is few, and opalescence is little |
| pH | 7.24 | 6.37 | 7.0 |
| Color number | No. 7 | No. 8 | No. 6 |
Also can be used for the Radix Notoginseng total arasaponins is raw material, the preparation production technique of preparation XUESAITONG ZHUSHEYE.Be that Radix Notoginseng total arasaponins adds water for injection, mix and boil → add active carbon that filtration and fine straining → ultrafiltration → nanofiltration → adding sodium chloride are an amount of, regulate the pH value water and dilute in right amount, obtain XUESAITONG ZHUSHEYE.
Embodiment 3:
Raw material: Radix Notoginseng
Membrane material: the ultrafilter membrane material is for gathering mystery sulfone film, and molecular cut off is 100000, and version is rolled film; NF membrane material aromatic polyamide composite membrane, molecular cut off are 200.
An amount of needle-use activated carbon of Radix Notoginseng → pulverizing → ethanol lixiviate → go up macroporous resin column → peroxidating aluminum post → add, titanium rod filtrations → ultrafiltration → nanofiltration → refining is concentrated → drying → pulverizing → Radix Notoginseng total arasaponins highly finished product.
Cross flow filter is adopted in ultrafiltration, and the import of ultrafiltrate is pressed and is 0.2MPa, and liquid outlet pressure ratio inlet pressure is low, and the feed liquid flow velocity is 50mL/s, and the filter of ultrafiltration material is filtered into 93.31%; Feed temperature is 22 ℃; The pH value 7.14 of feed liquid; When feed liquid stock solution by ultrafiltration when a small amount of, adding purified water again, to be diluted to proportion be 1.03 to continue ultrafiltration, repeats ultrafiltration repeatedly; After technical process finishes, titanium rod filtrate, the surplus liquid of ultrafiltration and Radix Notoginseng total arasaponins highly finished product are compared:
| Each constituent content | Titanium rod filtrate | The surplus liquid of ultrafiltration | The Radix Notoginseng total arasaponins highly finished product |
| R1 | 6.4 | 5.3 | 6.5 |
| Rg1 | 28.8 | 23.6 | 29.5 |
| Rb1 | 31.2 | 40.1 | 32.1 |
| Visible foreign matters | The trace floccule | A small amount of floccule | No floccule |
| pH | 7.14 | 6.37 | 7.62 |
| Color number | No. 5 | No. 6 | No. 3 |
Also can be used for the Radix Notoginseng total arasaponins is raw material, the preparation production technique of preparation XUESAITONG ZHUSHEYE.Be that Radix Notoginseng total arasaponins adds water for injection, mix and boil → add active carbon that filtration and fine straining → ultrafiltration → nanofiltration → adding sodium chloride are an amount of, regulate the pH value water and dilute in right amount, obtain XUESAITONG ZHUSHEYE.
Embodiment 4:
Raw material: Radix Notoginseng:
Membrane material: the ultrafilter membrane material is a Kynoar, and molecular cut off is 30000, and version is rolled film; NF membrane material aromatic polyamide composite membrane, molecular cut off are 200.
An amount of needle-use activated carbon of Radix Notoginseng → pulverizing → ethanol lixiviate → go up macroporous resin column → peroxidating aluminum post → add, titanium rod filtrations → ultrafiltration → nanofiltration → refining is concentrated → drying → pulverizing → Radix Notoginseng total arasaponins highly finished product.
Cross flow filter is adopted in ultrafiltration, and the import of ultrafiltrate is pressed to 0.25MPa liquid outlet pressure ratio inlet pressure is low, and the feed liquid flow velocity is 13mL/s, and the filter of ultrafiltration material is filtered into 92.70%; Feed temperature is 22 ℃; The pH value 7.43 of feed liquid; When feed liquid stock solution by ultrafiltration when a small amount of, adding purified water again, to be diluted to proportion be 1.03 to continue ultrafiltration, repeats ultrafiltration repeatedly; After technical process finishes, titanium rod filtrate, the surplus liquid of ultrafiltration and Radix Notoginseng total arasaponins highly finished product are compared:
| Each constituent content | Titanium rod filtrate | The surplus liquid of ultrafiltration | The Radix Notoginseng total arasaponins highly finished product |
| R1 | 7.3 | 5.6 | 7.6 |
| Rg1 | 31.4 | 23.9 | 32.5 |
| Rb1 | 31.8 | 33.8 | 31.6 |
| Visible foreign matters | A small amount of floccule | The volume floccule | Little floccule |
| pH | 7.43 | 7.23 | 7.96 |
| Color number | No. 6 | No. 7 | No. 4 |
Also can be used for the Radix Notoginseng total arasaponins is raw material, the preparation production technique of preparation XUESAITONG ZHUSHEYE.Be that Radix Notoginseng total arasaponins adds water for injection, mix and boil → add active carbon that filtration and fine straining → ultrafiltration → nanofiltration → adding sodium chloride are an amount of, regulate the pH value water and dilute in right amount, obtain XUESAITONG ZHUSHEYE.
Claims (3)
1. the method for purification of a Radix Notoginseng total arasaponins; Comprise following technology: Radix Notoginseng → pulverizing → ethanol lixiviate → go up macroporous resin column → peroxidating aluminum post → titanium rod to filter → concentrate → drying → pulverizing → Radix Notoginseng total arasaponins is characterized in that the excellent back of filtering of titanium in the Radix Notoginseng total arasaponins production technology increases membrane ultrafiltration, nanofiltration operation; The operating condition of ultrafiltration, nanofiltration operation is following:
1) inlet hydraulic is 0.1～0.5Mpa;
2) the feed liquid flow velocity is 10～40ml/s;
3) feed temperature is 15～40 ℃;
4) when feed liquid stock solution is extremely a small amount of by ultrafiltration, add the purified water dilution again, repeat ultrafiltration repeatedly;
5) pH value of feed liquid is controlled at 6.0～7.5;
6) backwash: backwashing period is every batch, and backwashing time is 1.5h;
The molecular cut off of described ultrafilter membrane adopts 10000～100000Da, and the molecular cut off of NF membrane adopts 200～500Da.
2. the method for purification of Radix Notoginseng total arasaponins according to claim 1 is characterized in that: membrane structure employing hollow fiber ultrafiltration membrane, rolling or tubular ultra-filtration membrane, employing cross flow filter or employing dead-end filtration.
3. the method for purification of Radix Notoginseng total arasaponins according to claim 1 is characterized in that: ultrafilter membrane material employing polysulfones membrane material, polypropylene, composite polrvinyl chloride; The NF membrane material adopts aromatic polyamide composite membrane.
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Cited By (2)
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| CN103830298A (en) * | 2014-03-26 | 2014-06-04 | 南京中医药大学 | Method for preparing panax notoginseng saponins by adopting membrane coupling technology |
| CN104958336A (en) * | 2015-07-08 | 2015-10-07 | 成都易胜科生物科技有限公司 | Method for purifying panax notoginseng saponins by combining ultrafiltration and nanofiltration technologies |
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| CN101947250B (en) * | 2010-08-30 | 2013-12-18 | 戴群 | Energy-saving process for extracting and purifying panax notoginseng saponins |
| CN102908404A (en) * | 2011-08-02 | 2013-02-06 | 苏州宝泽堂医药科技有限公司 | Method for extracting total saponin from polygala aureocauda Dunn |
| CN102441016B (en) * | 2011-12-13 | 2014-05-14 | 广西梧州制药（集团）股份有限公司 | Concentration method of pseudo-ginseng total saponin extracting solution |
| CN102429942B (en) * | 2011-12-27 | 2014-05-21 | 广西梧州制药（集团）股份有限公司 | Freeze-drying method of pseudo-ginseng total saponin freeze-dried injection powder with filling amount more than 500 mg |
| CN102585029B (en) * | 2012-03-08 | 2014-03-12 | 玉溪市维和生物技术有限责任公司 | Preparation method and application of physiologically active notoginseng polysaccharide |
| CN110663786A (en) * | 2019-11-20 | 2020-01-10 | 云南省农业科学院农产品加工研究所 | Processing method of pseudo-ginseng flower leaf tea beverage |
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