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 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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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000003018 immunoassay Methods 0.000 title claims abstract 3
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 238000010992 reflux Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000009833 condensation Methods 0.000 claims abstract description 18
- 230000005494 condensation Effects 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000009835 boiling Methods 0.000 claims abstract description 8
- 239000001509 sodium citrate Substances 0.000 claims abstract description 8
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 8
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract 6
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 claims description 10
- 239000003638 chemical reducing agent Substances 0.000 claims 1
- 239000012528 membrane Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 23
- 238000009826 distribution Methods 0.000 abstract description 12
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000012295 chemical reaction liquid Substances 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000084 colloidal system Substances 0.000 description 17
- 239000010931 gold Substances 0.000 description 17
- 229910052737 gold Inorganic materials 0.000 description 17
- 239000000203 mixture Substances 0.000 description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 238000005485 electric heating Methods 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- 239000000376 reactant Substances 0.000 description 6
- 230000015271 coagulation Effects 0.000 description 5
- 238000005345 coagulation Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000007667 floating Methods 0.000 description 4
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 4
- 230000002829 reductive effect Effects 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 2
- 239000001263 FEMA 3042 Substances 0.000 description 2
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 2
- 229940033123 tannic acid Drugs 0.000 description 2
- 235000015523 tannic acid Nutrition 0.000 description 2
- 229920002258 tannic acid Polymers 0.000 description 2
- 239000006059 cover glass Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
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- 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
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)
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510126133 CN1979166A (en) | 2005-11-30 | 2005-11-30 | A process for preparing nano colloidal gold for immunoassay and reaction device thereof |
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|---|---|---|---|
| CN 200510126133 CN1979166A (en) | 2005-11-30 | 2005-11-30 | A process for preparing nano colloidal gold for immunoassay and reaction device thereof |
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| CN1979166A true CN1979166A (en) | 2007-06-13 |
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Cited By (5)
| 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 |
-
2005
- 2005-11-30 CN CN 200510126133 patent/CN1979166A/en active Pending
Cited By (9)
| 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 |
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Open date: 20070613 |