CN1979166A - Process for nano colloid gold for immune detection and reaction apparatus therefor - Google Patents
Process for nano colloid gold for immune detection and reaction apparatus therefor Download PDFInfo
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- CN1979166A CN1979166A CN 200510126133 CN200510126133A CN1979166A CN 1979166 A CN1979166 A CN 1979166A CN 200510126133 CN200510126133 CN 200510126133 CN 200510126133 A CN200510126133 A CN 200510126133A CN 1979166 A CN1979166 A CN 1979166A
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Abstract
The invention relates to a technology method and reacting device for making detection using nanometer colloidal gold that includes the following steps: setting material intake on reacting device, and having sealing cover, whisking device is set in the reacting device, and condensate reflux unit is set on top, heater is set on the bottom of the reactor and the four sides of bottom to form heating area to take equal heating to reaction liquid; adding auric chloride acid solution into reacting device to take heating, starting whisking device and taking cooling by using condensate reflux unit; after solution boiling, adding citric acid-3-natrium solution, after boiling for 10 minutes, stop heating; cooling and filtering to gain colloidal gold. The invention could gain the colloidal gold that has good sphericity and size distribution.
Description
Technical field
The present invention relates to a kind of new synthetic immunity process and the reaction unit thereof of nano colloid gold.
Background technology
The existing preparation immune detection of generally using is trisodium citrate reduction chlorauric acid solution method with the technology of nano colloid gold.In the course of reaction, and traditional handicraft exist such as reaction system be heated in inhomogeneous, the heating process moisture evaporation serious, stir defectives such as inhomogeneous, greatly influenced size difference, sphericity, size distribution of the colloid gold particle that is obtained etc., be easy to generate " doing ".
Summary of the invention
The purpose of this invention is to provide a kind of process for preparing immune detection with nano colloid gold, the collaurum that is obtained is compared all with the prepared collaurum of current methods at aspects such as grain size difference, sphericity, size distribution and is improved.
Another object of the present invention provides a kind of reaction unit for preparing immune detection with nano colloid gold, and this reaction unit can make reactant liquor be heated evenly, stir, and keeps moisture non-volatile.
For achieving the above object, the present invention is by the following technical solutions:
A kind of process for preparing immune detection with nano colloid gold, this method comprises the steps:
(1), adopts reaction unit, this reaction unit is provided with charging aperture, and is furnished with airtight lid, in reaction unit, be provided with stirring apparatus, the top is provided with condensation reflux unit, the bottom of reactor and the wall on the bottom are provided with well heater to form the heating zone, and the reaction zone that reactant liquor is housed in this heating zone coating reaction device is to form the even heating to reactant liquor;
(2), chlorauric acid solution is joined the reaction unit, cover the charging aperture lid simultaneously, chlorauric acid solution is heated, open stirring apparatus simultaneously, and utilize condensation reflux unit to cool off by well heater from charging aperture;
(3), the heating chlorauric acid solution to boiling, add the reductive agent citric acid three sodium solution rapidly, cover the charging aperture lid simultaneously, keep the solution boiling after 10 minutes, stop heating;
(4), treat that solution cooling back by membrane filtration, obtains colloidal gold solution.
Compare with classic method, the mol ratio of the chlorauric acid solution concentration that the inventive method adopted, gold chloride and trisodium citrate, reaction time, temperature of reaction etc. are all identical, difference is that the inventive method adopts evenly heating, even alr mode, and adopts airtight condensing reflux.Since at chlorauric acid solution and citric acid three sodium solution in course of reaction, heating and alr mode have a significant impact product quality, therefore, and for obtaining high-quality product, must make reactant liquor be heated evenly, stir, thereby reductive agent and gold chloride are fully mixed; And employing condensing reflux mode, the leakproofness that keeps simultaneously reaction system to greatest extent, make the water vapor condensing reflux in condensation reflux unit that produces in the heating process can prevent to form so-called " doing ", thereby avoid colloid gold particle to condense to reaction system.
The used reaction unit of a kind of process of the present invention, this reaction unit is provided with charging aperture, and is furnished with airtight lid, in reaction unit, be provided with stirring apparatus, its top is provided with condensation reflux unit, the bottom of reaction unit and the wall on the bottom are provided with well heater to form the heating zone, and the reaction zone that reactant liquor is housed in this heating zone coating reaction device is to form the even heating to reactant liquor.
The top assembling condensation reflux unit of reaction unit, charging aperture is furnished with airtight lid simultaneously, the leakproofness that farthest keeps reaction system, can make the water vapor that produces in the heating process in condensation reflux unit, be back in the reaction system after the condensation, prevent to form so-called " doing ", thereby avoid colloid gold particle to condense; Utilize stirring apparatus fully to stir in the course of reaction, be beneficial to reductive agent and gold chloride fully mixes; The diapire of reaction unit and the wall on the bottom are provided with well heater, just at the diapire of reaction unit and the wall on the bottom electric jacket are housed, uniformity of temperature profile when heating.
Adopting three mouthfuls of glass flask is reactor, and the wall on bottom and the bottom heats with electric jacket, uniformity of temperature profile; Assembling condensation reflux unit in top farthest keeps the leakproofness of reaction system simultaneously, and the water vapor that produces in the heating process is back to behind condensing tube condensation in the reaction system, prevent to form so-called " doing " thus cause colloid gold particle to condense; Utilize the glass stirring arm fully to stir in the course of reaction, be beneficial to reductive agent and gold chloride fully mixes.
In the employed reaction unit of process of the present invention, described condensation reflux unit is to be made of serpentine condenser and cooling tube, one end of this serpentine condenser communicates with the reaction unit top, and the other end communicates with atmosphere, and this cooling tube is enclosed in around the serpentine condenser.
The invention has the advantages that: reaction unit of the present invention efficiently solve the inequality of being heated in the traditional handicraft, moisture evaporation serious, stir unequal defective.The prepared collaurum of process of the present invention has advantages such as good sphericity, narrow diameter distribution, particle size difference be little.
Description of drawings
Fig. 1 is a kind of reaction unit of preparation collaurum, and the symbol among Fig. 1 is represented respectively: 1, and---iron stand, 2---------there-necked flask, 4 is starched electric heating thermal insulation cover, 3,5---serpentine condenser, 6---cooling tube by mechanical raking;
Fig. 2 is the TEM photo of the particle diameter 5nm colloid gold particle of embodiment 1;
Fig. 3 is the TEM photo of the particle diameter 15nm colloid gold particle of embodiment 2;
Fig. 4 is the particle diameter 5nm collaurum size distribution statistical graph of embodiment 1;
Fig. 5 is the particle diameter 15nm collaurum size distribution statistical graph of embodiment 2;
Fig. 6 is the collaurum TEM photo of comparative example 1;
Fig. 7 is the collaurum TEM photo of comparative example 2.
Embodiment
Reaction unit of the present invention can adopt a kind of device as shown in Figure 1: adopt there-necked flask 3 to be reactor, there-necked flask 3 places on the electric heating thermal insulation cover 2.Electric heating thermal insulation cover 2 is to be provided with electric heater (diagram does not mark) in the container of heating medium is housed, and makes the heating medium heating by electric heater, thereby form the electric heating thermal insulation cover there-necked flask 3 is evenly heated.At the left side of Fig. 1 there-necked flask 3 mouth, just the charging aperture of reaction unit is furnished with glass stopper, to reduce the volatilization of moisture; Mouth on there-necked flask 3 the right is equipped with condensation reflux unit, this device is made of serpentine condenser 5 and cooling tube 6, serpentine condenser 5 is snakelike shape and coiling from bottom to top (figure does not mark snakelike shape), the one end communicates with the right mouth of there-necked flask 3, the other end communicates with atmosphere, cooling tube 6 be enclosed in serpentine condenser 5 around, and be provided with out, water inlet; The middle port of there-necked flask 3 clogs with stopper, and beyond the Great Wall glass machinery stirring arm 4 is installed.There-necked flask 3, electric heating thermal insulation cover 2 are assemblied on the iron stand 1.
As shown in Figure 1, transfer pipet is accurately measured the chlorauric acid solution of 1ml quality percentage composition 1% in there-necked flask 3, and thin up is to 100mL; There-necked flask 3 places on the electric heating thermal insulation cover 2, glass machinery stirring arm 4 is installed on the stopper of the middle port of Fig. 1 there-necked flask 3, at the right of there-necked flask 3 mouth assembling condensation reflux unit, mouth is added a cover glass stopper on the left side of there-necked flask 3, to reduce the volatilization of moisture; Start mechanical glass stirring arm 4 and feed tap water and cool off, begin to be heated to the solution boiling, mouthful add the citric acid three sodium solutions of a certain amount of quality percentage compositions 1% then rapidly by there-necked flask 3 left sides, then glass stopper beyond the Great Wall immediately to serpentine condenser 5; Keep the solution boiling after 10 minutes, stop heating and remove experimental provision.Treat the MILLI-Q membrane filtration of solution cooling back, solution is moved liquid to volumetric flask, promptly get colloidal gold solution with 0.22nm.It is little that TEM photo such as Fig. 2, the Fig. 3 of colloid gold particle by the method preparation, visible product have extraordinary sphericity, narrow diameter distribution, particle size difference.
Embodiment
Embodiment 1, adopt reaction unit shown in the present to be prepared, reaction conditions is: temperature of reaction is that 60 ℃, stir speed (S.S.) are 300rpm, quality percentage composition 1% trisodium citrate addition 4mL, 0.025mol/L K
2C0
3Addition is 0.6mL, and the addition of quality percentage composition 1% tannic acid is 0.6mL, quality percentage composition 1%HAuCl
4Addition is that 1mL, reaction time are 10min.
Test result: collaurum TEM photo as shown in Figure 2, colloid gold particle has extraordinary sphericity, narrow diameter distribution, the particle size difference is little.Colloidal gold solution surface no floating thing (nothing is done) is not found the coagulation phenomenon; Measuring the collaurum mean grain size is 5.07nm, and Fig. 4 is size distribution figure; 4 ℃ of sealings of this collaurum are placed and were not occurred the coagulation phenomenon in 30 days.
Embodiment 2, be prepared with reaction unit shown in the present, reaction conditions is: temperature of reaction is that 100 ℃, reaction time are that 10min, stir speed (S.S.) are 300rpm, quality percentage composition 1% trisodium citrate addition 12.2mL, quality percentage composition 1%HAuCl
4Addition is 3mL.
Test result: collaurum TEM photo as shown in Figure 3, colloid gold particle has extraordinary sphericity, narrow diameter distribution, the particle size difference is little.Colloidal gold solution surface no floating thing (nothing is done) is not found the coagulation phenomenon.Measuring the collaurum mean grain size is 14.88nm, and Fig. 5 is size distribution figure; 4 ℃ of sealings of this collaurum are placed and were not occurred the coagulation phenomenon in 30 days.
Comparative example
Comparative example 1, adopt conventional preparation method, use reaction vessel such as beaker directly on electric furnace, to heat, do not seal reflux.Reaction conditions is: temperature of reaction is that 60 ℃, stir speed (S.S.) are 300rpm, quality percentage composition 1% trisodium citrate addition 4mL, 0.025mol/L K
2CO
3Addition is 0.6mL, and the addition of quality percentage composition 1% tannic acid is 0.6mL, quality percentage composition 1%HAuCl
4Addition is that 1mL, reaction time are 10min.
Test result: collaurum TEM photo as shown in Figure 6, it is inferior spherical that colloid gold particle is, the size distribution broad, the particle size difference is obvious, has the bulky grain of gathering to exist.There is floating thing on the colloidal gold solution surface, in the form of sheets; 4 ℃ of sealings of this collaurum are placed and were not occurred the coagulation phenomenon in 30 days.
Comparative example 2, adopt conventional preparation method, use reaction vessel such as beaker directly on electric furnace, to heat, do not seal reflux.Reaction conditions is: temperature of reaction is that 100 ℃, reaction time are that 10min, stir speed (S.S.) are 300 rpm, quality percentage composition 1% trisodium citrate addition 12.2mL, quality percentage composition 1%HAuCl
4Addition is 3mL.
Test result: collaurum TEM photo as shown in Figure 7, colloid gold particle is irregular sphere, the particle size difference is bigger, has the bulky grain of gathering to exist.There is floating thing on the colloidal gold solution surface, in the form of sheets; 4 ℃ of sealings of this collaurum are placed after 30 days and deposited phenomenon occurred.
Claims (3)
1, a kind of process for preparing immune detection with nano colloid gold, this method comprises the steps:
(1), adopts reaction unit, this reaction unit is provided with charging aperture, and is furnished with airtight lid, in reaction unit, be provided with stirring apparatus, the top is provided with condensation reflux unit, the bottom of reactor and the wall on the bottom are provided with well heater to form the heating zone, and the reaction zone that reactant liquor is housed in this heating zone coating reaction device is to form the even heating to reactant liquor;
(2), chlorauric acid solution is joined the reaction unit, cover the charging aperture lid simultaneously, chlorauric acid solution is heated, open stirring apparatus simultaneously, and utilize condensation reflux unit to cool off by well heater from charging aperture;
(3), the heating chlorauric acid solution to boiling, add the reductive agent citric acid three sodium solution rapidly, cover the charging aperture lid simultaneously, keep the solution boiling after 10 minutes, stop heating;
(4), treat that solution cooling back by membrane filtration, obtains colloidal gold solution.
2, the used reaction unit of a kind of method of claim 1, it is characterized in that: this reaction unit is provided with charging aperture, and is furnished with airtight lid, in reaction unit, be provided with stirring apparatus, its top is provided with condensation reflux unit, the bottom of reaction unit and the wall on the bottom are provided with well heater to form the heating zone, and the reaction zone that reactant liquor is housed in this heating zone coating reaction device is to form the even heating to reactant liquor.
3, reaction unit according to claim 2 is characterized in that: described condensation reflux unit is to be made of serpentine condenser and cooling tube, and an end of this serpentine condenser communicates with the reaction unit top, the other end communicates with atmosphere; This cooling tube be enclosed in serpentine condenser around.
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| CN 200510126133 CN1979166A (en) | 2005-11-30 | 2005-11-30 | Process for nano colloid gold for immune detection and reaction apparatus therefor |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108872112A (en) * | 2018-07-07 | 2018-11-23 | 北京建筑大学 | The detection method of lead ion |
| CN111053908A (en) * | 2013-05-03 | 2020-04-24 | 西莱克塔生物科技公司 | Administration combination for reducing undesired humoral immune responses |
| US11633422B2 (en) | 2014-09-07 | 2023-04-25 | Selecta Biosciences, Inc. | Methods and compositions for attenuating anti-viral transfer vector immune responses |
| US11717569B2 (en) | 2011-04-29 | 2023-08-08 | Selecta Biosciences, Inc. | Tolerogenic synthetic nanocarriers |
-
2005
- 2005-11-30 CN CN 200510126133 patent/CN1979166A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11717569B2 (en) | 2011-04-29 | 2023-08-08 | Selecta Biosciences, Inc. | Tolerogenic synthetic nanocarriers |
| US11779641B2 (en) | 2011-04-29 | 2023-10-10 | Selecta Biosciences, Inc. | Tolerogenic synthetic nanocarriers for allergy therapy |
| CN111053908A (en) * | 2013-05-03 | 2020-04-24 | 西莱克塔生物科技公司 | Administration combination for reducing undesired humoral immune responses |
| CN111068061A (en) * | 2013-05-03 | 2020-04-28 | 西莱克塔生物科技公司 | Administration combination for reducing undesired humoral immune responses |
| US11633422B2 (en) | 2014-09-07 | 2023-04-25 | Selecta Biosciences, Inc. | Methods and compositions for attenuating anti-viral transfer vector immune responses |
| CN108872112A (en) * | 2018-07-07 | 2018-11-23 | 北京建筑大学 | The detection method of lead ion |
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Open date: 20070613 |