CN109986073A - A kind of Aurum clusters method for quickly purifying based on ultrafiltration - Google Patents
A kind of Aurum clusters method for quickly purifying based on ultrafiltration Download PDFInfo
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- CN109986073A CN109986073A CN201910037777.8A CN201910037777A CN109986073A CN 109986073 A CN109986073 A CN 109986073A CN 201910037777 A CN201910037777 A CN 201910037777A CN 109986073 A CN109986073 A CN 109986073A
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- aurum clusters
- ultrafiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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Abstract
The present invention relates to a kind of Aurum clusters method for quickly purifying based on ultrafiltration, include the following steps: that the untreated crude product in solution 4mL of Aurum clusters is placed in the inner tube of super filter tube (specification 3KDa), then super filter tube low speed refrigerated centrifuge is placed in be centrifuged, revolving speed is 3500-4000 revs/min, it is 100-180 minutes a length of when centrifugation, 4 DEG C of temperature, in centrifugal process, the impurity such as the small molecule in solution are filled into outer tube under the action of the centrifugal force, and Aurum clusters after purification are obtained in inner tube.This have the characteristics that operation it is convenient, rapidly and efficiently, it is environmentally protective.
Description
Technical field
The invention belongs to material purifying field, in particular to a kind of method for quickly purifying of the Aurum clusters based on ultrafiltration.
Background technique
Aurum clusters typically refer to size in 2nm gold nano-material below.Aurum clusters have significant quantum size effect,
The discrete electrons structure at cluster core center is made it have, therefore spectrum shows the single electron transition of similar molecule, rather than it is general
The surface plasma body resonant vibration of logical nano material.The unique geometry of Aurum clusters and electronic structure make it produce many interesting spies
Property, such as chirality, magnetism, redox characteristic, photovoltaic property are (referring to Santosh Kumar et.al, Water-soluble
Au25(Capt)18nanoclusters:synthesis,thermal stability,and optical properties,
Nanoscale,2012,4,4222).These characteristics make Aurum clusters be widely used in many aspects, in recent years each neck
Domain scientists have carried out fruitful exploration in synthesis characterization and application aspect.
There are two types of the most common synthetic methods of Aurum clusters: carrying out redox reaction by end-capping reagent and reducing agent to make
It is standby；Large scale gold nano grain performs etching under alkaline condition.First method have been achieved for remarkable effect and increasingly at
It is ripe, it is the most common preparation method in current experiment room.The chemical reduction reaction carried out under end-capping reagent and reducing agent existence condition
Three valence state gold ions are reduced into monovalence even zero-valent state, to obtain stable Aurum clusters.(referring to Su Lei, ratio probes examination
Visualization identification of the paper to glucose in human serum, China Science & Technology University's master thesis, 2018)
Aurum clusters are widely used for the fields such as analysis detection and biomedicine at present.The object of analysis detection includes gold
Belong to ion (such as Hg2+、Pb2+、Cu2+), small organic molecule (such as ascorbic acid, dopamine, glucose, cholesterol), polypeptide, ammonia
Base acid (such as cysteine, glutathione, ATP), protein molecular and enzyme (referring to Xu Chao, based on Aurum clusters multi-mode at
The correlation research of picture and markers in diagnosis, Beijing University of Technology Ph.D. Dissertation, 2017).Field of biomedicine
Using including based on (the ginseng such as cell in vitro horizontal imaging and living body horizontal imaging, drug transport, enzymatic activity regulation, biomarker
See Zhang Qian, nano Au particle, the synthesis of nano golden cluster and its modification research to glucose oxidase, Sichuan Agricultural University are large
Bachelorship paper, 2011).
Containing impurity such as a large amount of residual reactants in the Aurum clusters crude product in solution of synthesis, it is needed to be purified.When
It is preceding it has been reported that purification process include organic solvent precipitation method, dialysis, electrophoresis, liquid chromatography separation etc..It answers at present
With it is wide be polyacrylamide gel electrophoresis, principle is contained in the size of Aurum clusters and electrically charged amount and thick solution
Impurity it is different, therefore migration velocity in the electric field has differences and then realizes separation, but this method also needs after purification
Carry out the subsequent processings such as colloidal sol (referring to Gong Dejun etc., preparation, property and the application of chiral Aurum clusters, chemical progress, 2015).
In addition, dialysis is also more common, according to the dialysis membrane of different Aurum clusters size selection different molecular weights, golden group is generally required
The solution of cluster crude product is dialysed a few days using dialysis membrane, and replaces a ultrapure water at regular intervals (referring to Su Lei, ratio spy
Visualization identification of the needle test paper to glucose in human serum, China Science & Technology University's master thesis, 2018).It is above-mentioned this
There is the problems such as time-consuming, cumbersome, at high cost, low yield, dependence organic reagent (pollution environment) in various degree in a little methods.
Summary of the invention
The purpose of the present invention is improving the purification process of existing Aurum clusters, it is quickly pure to provide a kind of Aurum clusters based on ultrafiltration
Change new method.Specific technical solution is as follows:
Aurum clusters (synthesizing through reduction method) untreated crude product in solution is placed in the inner tube of super filter tube that (specification is
3kDa), super filter tube is then placed in low speed refrigerated centrifuge to be centrifuged, revolving speed is 3500-4000 revs/min, is centrifuged duration
It is 100-180 minutes, 4 DEG C of temperature, in centrifugal process, the impurity such as small molecule in solution are filled into outer tube under the action of the centrifugal force
In, Aurum clusters after purification are obtained in inner tube.
Above-mentioned technical proposal have the characteristics that operation it is convenient, rapidly and efficiently, it is environmentally protective.Simultaneously as most of solvent
It is filtered to outer tube with impurity, the Aurum clusters in inner tube are significantly concentrated.Therefore, above-mentioned Jin Tuanchun provided by the invention
Change method has concentrated effect simultaneously.
Detailed description of the invention
Fig. 1 preferred embodiments Aurum clusters before purification after in super filter tube comparison photo (left side be ultrafiltration before, the right is super
After filter)；
Fig. 2 preferred embodiments Aurum clusters before purification after ultraviolet spectrogram (for red for before purification, black is after purification)；
The TEM figure of Fig. 3 preferred embodiments Aurum clusters after purification；
1 Aurum clusters of Fig. 4 embodiment before purification after in super filter tube comparison photo (left side be ultrafiltration before, the right is ultrafiltration
Afterwards)；
1 Aurum clusters of Fig. 5 embodiment before purification after ultraviolet spectrogram (for red for before purification, black is after purification)；
2 Aurum clusters of Fig. 6 embodiment before purification after in super filter tube comparison photo (left side be ultrafiltration before, the right is ultrafiltration
Afterwards)；
2 Aurum clusters of Fig. 7 embodiment before purification after ultraviolet spectrogram (for red for before purification, black is after purification)；
Technology Roadmap Fig. 8 of the invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the present invention is made into one below in conjunction with attached drawing
Step ground detailed description.
Preferred embodiments
The technical solution of the present embodiment is as follows: the inner tube of super filter tube is added in untreated Aurum clusters crude product in solution 4mL
In (specification 3kDa), super filter tube is placed in low speed refrigerated centrifuge and is centrifuged, 4000 revs/min of revolving speed, be centrifuged duration
100min, 4 DEG C of temperature.Fig. 1 shows that the Aurum clusters liquor capacity after centrifugation in inner tube containing purified concentration is 150uL or so,
Most of solvent and small molecular weight impurity in former solvent have been centrifuged in outer tube.Fig. 2 shows, before purification ultraviolet spectra medium wave
There are a large amount of miscellaneous peak in long 200-300nm ranges, show in Aurum clusters crude product in solution there are plurality of impurities, and Aurum clusters
Characteristic peak (near 650nm) it is weaker；Impurity peaks all disappear after purification, while the characteristic peak of Aurum clusters is remarkably reinforced, display
Impurity is filtered, and has good purification effect.Fig. 3 gives the transmission electron microscope of preferred embodiments Aurum clusters after purification
(TEM) figure shows near Aurum clusters particle diameter distribution 2nm, is uniformly dispersed, other impurities are not observed.
Embodiment 1
The technical solution of the present embodiment is as follows: untreated Aurum clusters crude product in solution 4mL is added to the interior of super filter tube
In pipe (specification 3kDa), super filter tube is placed in low speed refrigerated centrifuge and is centrifuged, 3800 revs/min of revolving speed, is centrifuged duration
160min, 4 DEG C of temperature.Fig. 4 shows that the Aurum clusters liquor capacity after centrifugation in inner tube containing purified concentration is 150uL or so,
Most of solvent and small molecular weight impurity in former solvent have been centrifuged in outer tube.Fig. 5 shows, before purification ultraviolet spectra medium wave
There are a large amount of miscellaneous peak in long 200-300nm ranges, show in Aurum clusters crude product in solution there are plurality of impurities, and Aurum clusters
Characteristic peak (near 650nm) it is weaker；Impurity peaks all disappear after purification, while the characteristic peak of Aurum clusters is remarkably reinforced, display
Impurity is filtered, and has good purification effect.
Embodiment 2
The technical solution of the present embodiment is as follows: untreated Aurum clusters crude product in solution 4mL is added to the interior of super filter tube
In pipe (specification 3kDa), super filter tube is placed in low speed refrigerated centrifuge and is centrifuged, 3500 revs/min of revolving speed, is centrifuged duration
100min, 4 DEG C of temperature.Fig. 4 shows that the Aurum clusters liquor capacity after centrifugation in inner tube containing purified concentration is 150uL or so,
Most of solvent and small molecular weight impurity in former solvent have been centrifuged in outer tube.Fig. 5 shows, before purification ultraviolet spectra medium wave
There are a large amount of miscellaneous peak in long 200-300nm ranges, show in Aurum clusters crude product in solution there are plurality of impurities, and Aurum clusters
Characteristic peak (near 650nm) it is weaker；Impurity peaks all disappear after purification, while the characteristic peak of Aurum clusters is remarkably reinforced, display
Impurity is filtered, and has good purification effect.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, therefore equivalent changes made in accordance with the claims of the present invention, is still within the scope of the present invention.
Claims (4)
1. a kind of Aurum clusters method for quickly purifying based on ultrafiltration, which comprises the steps of: through reduction method synthesis
The untreated crude product in solution of Aurum clusters is placed in the inner tube of super filter tube, and super filter tube is then placed in centrifuge and is centrifuged,
Revolving speed is 3500-4000 revs/min, and when centrifugation is 100-180 minutes a length of, in centrifugal process, the impurity such as small molecule in solution
It is filled into outer tube under the action of the centrifugal force, Aurum clusters after purification is obtained in inner tube.
2. the Aurum clusters method for quickly purifying according to claim 1 based on ultrafiltration, it is characterised in that: the crude product
Solution 4mL, 4 DEG C of temperature when centrifugation.
3. according to the method described in claim 1, it is characterized by: the super filter tube specification is 3KDa.
4. according to the method described in claim 1, it is characterized by: the centrifugation uses low speed refrigerated centrifuge.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102188447A (en) * | 2010-03-16 | 2011-09-21 | 博安兄弟制药（中国）有限公司 | Preparation method for cerebroprotein hydrolysate in piracetam cerebroprotein hydrolysate tablets |
| CN107296961A (en) * | 2017-07-17 | 2017-10-27 | 中国药科大学 | A kind of conjugate of anti-human DLL4 monoclonal antibodies and adriamycin |
| CN107684560A (en) * | 2016-08-05 | 2018-02-13 | 深圳深见医药科技有限公司 | Material containing Aurum clusters is preparing the application in preventing and treating alzheimer medicine |
| JP2018127712A (en) * | 2017-02-10 | 2018-08-16 | 住友電気工業株式会社 | Method for producing copper nanoink |
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2019
- 2019-01-15 CN CN201910037777.8A patent/CN109986073B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102188447A (en) * | 2010-03-16 | 2011-09-21 | 博安兄弟制药（中国）有限公司 | Preparation method for cerebroprotein hydrolysate in piracetam cerebroprotein hydrolysate tablets |
| CN107684560A (en) * | 2016-08-05 | 2018-02-13 | 深圳深见医药科技有限公司 | Material containing Aurum clusters is preparing the application in preventing and treating alzheimer medicine |
| JP2018127712A (en) * | 2017-02-10 | 2018-08-16 | 住友電気工業株式会社 | Method for producing copper nanoink |
| CN107296961A (en) * | 2017-07-17 | 2017-10-27 | 中国药科大学 | A kind of conjugate of anti-human DLL4 monoclonal antibodies and adriamycin |
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