US4396528A
Expired / Lapsed
US
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Fluorescent composition, a process for synthesizing the fluorescent composition
Assignee: Varian Inc
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Filing: 1981-06-09
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Granted: 1983-08-02
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Expires: 2001-06-09
Abstract
Abstract A fluorescent composition useful in thin-layer chromatography comprises an inert porous particle having a fluorescent material fixedly attached by covalent chemical bonding to the surface thereof. A process for synthesizing this fluorescent composition is disclosed. A method for detecting the radioactivity of a radioactive species using a cell packed with such a fluorescent composition is also disclosed.
Inventors
- 👤 Seth R. Abbott
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 05:11
CPC Classifications
C; C09; C09K; C09K11/00; C09K11/02; C09K11/025; G; G01; G01N; G01N30/00; G01N30/90; G01N30/92; G01N30/93; G01T; G01T1/00; G01T1/003; G01T1/16; G01T1/20; G01T1/203
Claims Analysis
Total Claims: 29
Claim 1
Independent Claim
127 words
A process for the manufacture of a fluorescent composition comprising an inert porous particle having a size of about 5 to 20 microns, and a fluorescent material; said fluorescent material being fixedly attached by covalent chemical bonding to the surface of said particles; wherein said particle is microparticulate silica; said process comprising steps of: (a) reacting at room temperature an amine linking agent with an aqueous slurry of said silica whereby there is formed an intermediate product consisting of said amine linking agent covalently bonded to said silica; (b) recovering, washing and drying said intermediate product; (c) reacting at room temperature a slurry of the dried intermediate product with said fluorescent material whereby said fluorescent composition is produced; and (d) recovering, washing and drying said fluorescent composition.
Claim 2
Dependent Claim
127 words
A process for the manufacture of a fluorescent composition comprising an inert porous particle having a size of about 5 to 20 microns, and a fluorescent material; said fluorescent material being fixedly attached by covalent chemical bonding to the surface of said particles; wherein said particle is microparticulate silica; said process comprising steps of: (a) reacting at room temperature an amine linking agent with an aqueous slurry of said silica whereby there is formed an intermediate product consisting of said amine linking agent covalently bonded to said silica; (b) recovering, washing and drying said intermediate product; (c) reacting at room temperature a slurry of the dried intermediate product with said fluorescent material whereby said fluorescent composition is produced; and (d) recovering, washing and drying said fluorescent composition.
Claim 3
Dependent Claim
16 words
The process of claim 1 wherein said silica is high pressure liquid chromatography grade silica gel.
Claim 4
Dependent Claim
17 words
The process of claim 1 wherein said particle has a size of about 5 to 10 microns.
Claim 5
Dependent Claim
27 words
The process of claim 1 wherein the reaction of step (a) is carried out at about room temperature for a period of about 2 to 4 hours.
Claim 6
Dependent Claim
13 words
The process of claim 4 wherein the reaction time is about 3 hours.
Claim 7
Dependent Claim
32 words
The process of claim 1 wherein the reaction of step (c) is carried out at a temperature in the range of about 40° to 60° C. for about 1 to 3 hours.
Claim 8
Dependent Claim
54 words
The process of claim 1 wherein the slurry of step (c) is produced by adding the dried intermediate product to a mixture of a water-miscible organic solvent and a saturated aqueous solution, said organic solvent being present in an excess amount or in an about stoichiometrically equivalent amount with respect to said aqueous solution.
Claim 9
Dependent Claim
22 words
The process of claim 7 wherein said organic solvent is present in an about 4:1 ratio with respect to said aqueous solution.
Claim 10
Dependent Claim
11 words
The process of claim 8 wherein said organic solvent is acetonitrile.
Claim 11
Dependent Claim
16 words
The process of claim 7 wherein said saturated aqueous solution is water saturated with sodium bicarbonate.
Claim 12
Dependent Claim
22 words
The process of claim 1 wherein the reaction of step (c) is carried out at about 50° C. for about 2 hours.
Claim 13
Dependent Claim
13 words
The process of claim 1 wherein the amine linking agent is N-2-aminoethyl-3-aminopropyl trimethoxysilane.
Claim 14
Dependent Claim
14 words
The process of claim 1 wherein the amine linking agent is an amine-containing trialkoxysilane.
Claim 15
Dependent Claim
12 words
The process of claim 1 wherein said fluorescent composition is didansyl-N-2-aminoethyl-3-aminopropyl silica.
Claim 16
Dependent Claim
12 words
The process of claim 1 wherein said fluorescent material is dansyl chloride.
Claim 17
Dependent Claim
169 words
A fluorescent composition useful for detection of radioactive or non-fluorescent species by fluorescence, said composition comprising microparticulate silica having a size of about 5 to 20 microns, an amine linking agent fixedly attached by covalent chemical bonding to the surface of said microparticulate silica by reacting said microparticulate silica with said amine linking agent to form an intermediate product, and a fluorescent material fixedly attached to said amine linking agent by reacting said fluorescent material with the said intermediate product, said microparticulate silica-amine linking agent reaction comprising (a) reacting at room temperature an amine linking agent with an aqueous slurry of said silica whereby there is formed an intermediate product consisting of said amine linking agent covalently bonded to said silica and (b) recovering, washing and drying said intermediate product, and said fluorescent materialintermediate product reaction comprising (c) reacting at about room temperature a slurry of the dried intermediate product with said fluorescent material whereby said fluorescent composition is produced, and (d) recovering, washing and drying said fluorescent composition.
Claim 18
Dependent Claim
169 words
A fluorescent composition useful for detection of radioactive or non-fluorescent species by fluorescence, said composition comprising microparticulate silica having a size of about 5 to 20 microns, an amine linking agent fixedly attached by covalent chemical bonding to the surface of said microparticulate silica by reacting said microparticulate silica with said amine linking agent to form an intermediate product, and a fluorescent material fixedly attached to said amine linking agent by reacting said fluorescent material with the said intermediate product, said microparticulate silica-amine linking agent reaction comprising (a) reacting at room temperature an amine linking agent with an aqueous slurry of said silica whereby there is formed an intermediate product consisting of said amine linking agent covalently bonded to said silica and (b) recovering, washing and drying said intermediate product, and said fluorescent materialintermediate product reaction comprising (c) reacting at about room temperature a slurry of the dried intermediate product with said fluorescent material whereby said fluorescent composition is produced, and (d) recovering, washing and drying said fluorescent composition.
Claim 19
Dependent Claim
16 words
The fluorescent composition of claim 16 wherein said silica is high-pressure liquid chromatography grade silica gel.
Claim 20
Dependent Claim
18 words
The fluorescent composition of claim 16 wherein said silica has a size of about 5 to 10 microns.
Claim 21
Dependent Claim
14 words
The fluorescent composition of claim 16 wherein said amine linking agent is N-2-aminoethyl-3-aminopropyl trimethoxysilane.
Claim 22
Dependent Claim
20 words
The fluorescent composition of claim 19 wherein said fluorescent material is dansyl chloride, and said fluorescent composition is didansyl-N-2-aminoethyl-3-aminopropyl silica.
Claim 23
Dependent Claim
27 words
The composition of claim 16 wherein the reaction of step (a) is carried out at about room temperature for a period of about 2 to 4 hours.
Claim 24
Dependent Claim
13 words
The composition of claim 21 wherein the reaction time is about 3 hours.
Claim 25
Dependent Claim
54 words
The composition of claim 16 wherein the slurry of step (c) is produced by adding the dried intermediate product to a mixture of a water-miscible organic solvent and a saturated aqueous solution, said organic solvent being present in an excess amount or in an about stoichiometrically equivalent amount with respect to said aqueous solution.
Claim 26
Dependent Claim
22 words
The composition of claim 23 wherein said organic solvent is present in an about 4:1 ratio with respect to said aqueous solution.
Claim 27
Dependent Claim
11 words
The composition of claim 24 wherein said organic solvent is acetonitrile.
Claim 28
Dependent Claim
16 words
The composition of claim 23 wherein said saturated aqueous solution is water saturated with sodium bicarbonate.
Claim 29
Dependent Claim
22 words
The composition of claim 16 wherein the reaction of step (c) is carried out at about 50° C. for about 2 hours.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1986-08-01 | 1987-01-31 | 1987-08-02 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1990-08-01 | 1991-01-31 | 1991-08-02 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1994-08-01 | 1995-01-31 | 1995-08-02 | $7700.00 | Window Closed / Lapsed |