[go: up one dir, main page]

CN1979166A - A process for preparing nano colloidal gold for immunoassay and reaction device thereof - Google Patents

A process for preparing nano colloidal gold for immunoassay and reaction device thereof Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
reaction
reaction device
solution
heating
colloidal gold
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN 200510126133
Other languages
Chinese (zh)
Inventor
熊晓东
贺昕
梁敬博
陈峤
王胜国
张曦
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing General Research Institute for Non Ferrous Metals
Grikin Advanced Material Co Ltd
Original Assignee
Beijing General Research Institute for Non Ferrous Metals
Grikin Advanced Material Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Beijing General Research Institute for Non Ferrous Metals, Grikin Advanced Material Co Ltd filed Critical Beijing General Research Institute for Non Ferrous Metals
Priority to CN 200510126133 priority Critical patent/CN1979166A/en
Publication of CN1979166A publication Critical patent/CN1979166A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • Colloid Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

A process method for preparing nano colloidal gold for immunoassay and a reaction device thereof comprise (1) a reaction device is provided with a feed inlet and a closed cover body, a stirring device is arranged in the reaction device, a condensation reflux device is arranged at the top of the reaction device, heaters are arranged at the bottom of the reaction device and on the four walls of the bottom of the reaction device to form heating zones, and reaction liquid is uniformly heated; (2) adding the chloroauric acid solution into a reaction device, heating the chloroauric acid solution, opening a stirring device, and cooling by using a condensation reflux device; (3) heating the chloroauric acid solution to boiling, adding a trisodium citrate solution, boiling the solution for 10 minutes, and stopping heating; (4) and cooling and filtering to obtain the colloidal gold solution. The method solves the problems of uneven heating, serious moisture volatilization, uneven stirring and the like in the traditional process, prevents the generation of dry spots in the preparation of the colloidal gold, and the colloidal gold obtained by the method has good sphericity and particle size distribution and small particle size difference.

Description

A kind of process and reaction unit thereof for preparing immune detection with nano colloid gold
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、一种制备免疫检测用纳米胶体金的工艺方法,该方法包括下述步骤:1. A process for preparing nano colloidal gold for immunoassay, the method may further comprise the steps: (1)、采用反应装置,该反应装置设有进料口,并配有密闭盖体,在反应装置中设有搅拌装置,顶部设有冷凝回流装置,反应器的底部及底部上的四壁设有加热器以形成加热区,该加热区包覆反应装置中的装有反应液的反应区,以形成对反应液的均匀加热;(1), using a reaction device, the reaction device is provided with a feed inlet, and is equipped with a closed cover, a stirring device is provided in the reaction device, a condensation reflux device is provided at the top, the bottom of the reactor and the four walls on the bottom A heater is provided to form a heating zone, and the heating zone covers the reaction zone containing the reaction solution in the reaction device to form uniform heating of the reaction solution; (2)、从进料口将氯金酸溶液加入到反应装置中,同时盖合进料口盖体,通过加热器对氯金酸溶液进行加热,同时开通搅拌装置,及利用冷凝回流装置进行冷却;(2), join the chloroauric acid solution into the reaction device from the feed inlet, cover the feed inlet cover at the same time, heat the chloroauric acid solution through the heater, open the stirring device simultaneously, and utilize the condensation reflux device to carry out cool down; (3)、加热氯金酸溶液至沸腾后,迅速加入还原剂柠檬酸三钠溶液,同时盖合进料口盖体,保持溶液沸腾10分钟后,停止加热;(3), after heating the chloroauric acid solution to boiling, add reducing agent trisodium citrate solution rapidly, cover feed inlet cover body simultaneously, after keeping solution boiling for 10 minutes, stop heating; (4)、待溶液冷却后通过滤膜过滤,得到胶体金溶液。(4), after the solution is cooled, filter through a filter membrane to obtain a colloidal gold solution. 2、一种权利要求1的方法所用的反应装置,其特征在于:该反应装置设有进料口,并配有密闭盖体,在反应装置中设有搅拌装置,其顶部设有冷凝回流装置,反应装置的底部及底部上的四壁设有加热器以形成加热区,该加热区包覆反应装置中的装有反应液的反应区,以形成对反应液的均匀加热。2. A reaction device used in the method of claim 1, characterized in that: the reaction device is provided with a feed port, and is equipped with a closed cover, a stirring device is provided in the reaction device, and a condensation reflux device is provided at the top , The bottom of the reaction device and the four walls on the bottom are provided with heaters to form a heating zone, and the heating zone covers the reaction zone containing the reaction solution in the reaction device to form uniform heating of the reaction solution. 3、根据权利要求2所述的反应装置,其特征在于:所述的冷凝回流装置是由蛇形冷凝管和冷却管构成,该蛇形冷凝管的一端与反应装置顶部相通、另一端与大气相通;该冷却管包围在蛇形冷凝管的四周。3. The reaction device according to claim 2, characterized in that: the condensation reflux device is composed of a serpentine condenser pipe and a cooling pipe, one end of the serpentine condenser pipe communicates with the top of the reaction device, and the other end communicates with the atmosphere communicated; the cooling tube is surrounded by the serpentine condenser tube.
CN 200510126133 2005-11-30 2005-11-30 A process for preparing nano colloidal gold for immunoassay and reaction device thereof Pending CN1979166A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200510126133 CN1979166A (en) 2005-11-30 2005-11-30 A process for preparing nano colloidal gold for immunoassay and reaction device thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200510126133 CN1979166A (en) 2005-11-30 2005-11-30 A process for preparing nano colloidal gold for immunoassay and reaction device thereof

Publications (1)

Publication Number Publication Date
CN1979166A true CN1979166A (en) 2007-06-13

Family

ID=38130400

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 200510126133 Pending CN1979166A (en) 2005-11-30 2005-11-30 A process for preparing nano colloidal gold for immunoassay and reaction device thereof

Country Status (1)

Country Link
CN (1) CN1979166A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
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 Dosing Combinations for Reducing Undesirable 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
US12194078B2 (en) 2017-03-11 2025-01-14 Cartesian Therapeutics, Inc. Methods and compositions related to combined treatment with anti-inflammatories and synthetic nanocarriers comprising an immunosuppressant

Cited By (9)

* Cited by examiner, † Cited by third party
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 Dosing Combinations for Reducing Undesirable Humoral Immune Responses
CN111068061A (en) * 2013-05-03 2020-04-28 西莱克塔生物科技公司 Dosing Combinations for Reducing Undesirable Humoral Immune Responses
US12472167B2 (en) 2013-05-03 2025-11-18 Cartesian Therapeutics, Inc. Methods providing a therapeutic macromolecule and synthetic nanocarriers comprising immunosuppressant locally and concomitantly to reduce both Type 1 and Type IV hypersensitivity
US12508249B2 (en) 2013-05-03 2025-12-30 Cartesian Therapeutics Inc. Methods related to administering immunosuppressants and non-allergenic antigens to reduce or prevent anaphylaxis
US11633422B2 (en) 2014-09-07 2023-04-25 Selecta Biosciences, Inc. Methods and compositions for attenuating anti-viral transfer vector immune responses
US12194078B2 (en) 2017-03-11 2025-01-14 Cartesian Therapeutics, Inc. Methods and compositions related to combined treatment with anti-inflammatories and synthetic nanocarriers comprising an immunosuppressant
CN108872112A (en) * 2018-07-07 2018-11-23 北京建筑大学 The detection method of lead ion

Similar Documents

Publication Publication Date Title
CN102007073B (en) Alumina powder, process for production of the same, and resin compositions containing the same
CN108249806A (en) A kind of preparation method of hydrated calcium silicate early strength agent and a kind of self-compacting concrete
CN102173458A (en) Preparation method of bismuth ferrite nano powder
CN108033476A (en) A kind of preparation method of nano-calcium carbonate
CN1979166A (en) A process for preparing nano colloidal gold for immunoassay and reaction device thereof
CN101177301A (en) Method for preparing stabilized zirconia nanopowder
CN101884880A (en) Heat exchange stirrer
CN114210965B (en) Metallic silver and its preparation method and application
CN103979538B (en) A kind of method preparing micro-nano TiC/TiSi2 composite granule
CN103785853B (en) A kind of preparation method of hydridization carbon silver composite material
CN106554643A (en) The preparation method of high temperature resistant bismuth vanadium pigmentses
CN101357763A (en) Preparation method of high-purity ultrafine SiC powder
Zhang et al. Preparation and performance evaluation of paraffin@ SiO2 microencapsulated phase change material and its thermal insulation effect in architectural coatings
CN207169548U (en) A kind of powdery paints bonding machines
WO2024139112A1 (en) Process and system for preparing iron phosphate by using out-of-kettle circulating mixing and stirring
CN109249016A (en) A kind of 3D printing graphene/magnesium composite powder preparation method
CN108328661A (en) One step high temperature method prepares polyacrylic acid modified ferric oxide nano particl method
CN109592708A (en) The production method of colorant high Chromaticity power sulfuric acid process enamel grade titanium dioxide powder
CN104760972B (en) A kind of preparation method of same crystalline phase core shell structure beta-molecular sieve
CN103058204B (en) Heating method of steam direct connection making silica solution
CN109732099B (en) Preparation method of antioxidant micron copper
CN203764236U (en) Reaction device for preparing colloidal gold particles with different sizes
CN204381368U (en) Improve the Preparation equipment of the oxygen content of sub-micron nickel powder
CN204699437U (en) A kind of water cooling crystallization kettle
CN209599876U (en) A kind of photocuring 3D printing raw material mixing component and raw material heating device

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Open date: 20070613