IP Library Granted Patent US 12,416,638
Granted Patent B2
US 12,416,638 · App. 17/222,741 · Granted Sep 16, 2025

Methods for labeling amine-containing compounds

Inventors: Michael J. Kimzey (Oakland, CA); Alexander Gyenes (San Francisco, CA)
Assignee: Agilent Technologies, Inc.
G01N33/6809C07D207/46G01N33/582G01N33/6848G01N2400/10G01N2458/00Y10T436/143333Y10T436/173845
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Quick Facts
Patent No.
US 12,416,638
App. No.
17/222,741
Granted
Sep 16, 2025
Kind
B2
Abstract

The invention relates to an activated form of procaine, and the use of the activated procaine, or salts or solvates thereof, to label amine-containing compounds, such as N-glycans, amine-containing amino acids, amine-containing peptides, amine-containing proteins, or other amine-containing compounds in a sample. Use of activated procaine as a label allows for sensitive detection of compounds labeled with it by both fluorescence and mass spectrometry.

Claims (22)

1. A method for labeling and, optionally, analyzing, a N-glycan, amine-containing amino acid, amine-containing peptide, amine-containing protein, glycosylamine, or other amine-containing compound in a sample, said method comprising: (a) mixing said N-glycan, amine-containing amino acid, amine-containing peptide, amine-containing protein, glycosylamine, or other amine-containing compound in a solution with a labeling compound (“Activated Procaine”) with the structure

or a solvate or a salt of said labeling compound, thereby creating a labeling mixture, and

(b) conducting said labeling at a labeling temperature of between 10° C.±2° C. to 60° C.±2° C.,

thereby creating a labeled, fluorescent, mass spectrometry-active derivative of said N-glycan, of said amine-containing amino acid, of said amine-containing peptide, of said amine-containing protein, of said glycosylamine, or of said other amine-containing compound in said sample.

2. The method of claim 1 , wherein N-hydroxysuccinimide is present during said labeling of said N-glycan, amine-containing amino acid, amine-containing peptide, amine-containing protein, glycosylamine, or other amine-containing compound with said Activated Procaine or solvate or salt thereof.

3. The method of claim 1 , wherein said fluorescent, mass spectrometry-active derivative of said N-glycan, amine-containing amino acid, amine-containing peptide, amine-containing protein, glycosylamine, or other amine-containing compound is a fluorescent, mass spectrometry-active derivative of said N-glycan.

4. The method of claim 1 , wherein said fluorescent, mass spectrometry-active derivative of said N-glycan, amine-containing amino acid, amine-containing peptide, amine-containing protein, glycosylamine, or other amine-containing compound is a fluorescent, mass spectrometry-active derivative of said glycosylamine.

5. The method of claim 1 , wherein said labeling temperature is 45° C. to 55° C.

6. The method of claim 1 , wherein said labeling temperature is 50° C.±2° C.

7. The method of claim 1 , wherein said labeling temperature is 50° C.

8. The method of claim 1 , wherein said labeling is conducted by incubating said labeling mixture at said labeling temperature for 30 seconds to 5 minutes.

9. The method of claim 1 , wherein said labeling is conducted by incubating said labeling mixture at said labeling temperature for 1 minute ±15 seconds to 3 minutes ±15 seconds.

10. The method of claim 1 , wherein said labeling is conducted by incubating said labeling mixture at said labeling temperature for 1 minute ±15 seconds.

11. The method of claim 1 , wherein said labeling is conducted by heating said labeling mixture to a labeling temperature of 50° C.±2° C. and incubating said labeling mixture at said labeling temperature of 50° C.±2° C. for 1 minute ±15 seconds to 3 minutes ±15 seconds.

12. The method of claim 1 , wherein said labeling is conducted by heating said labeling mixture to a labeling temperature of 50° C.±2° C. and incubating said labeling mixture at said labeling temperature of 50° C.±2° C. for 1 minute ±15 seconds.

13. The method of claim 1 , wherein said labeling is conducted by heating said labeling mixture to a labeling temperature of 50° C. and incubating said labeling mixture at said labeling temperature of 50° C. for 1 minute ±15 seconds.

14. The method of claim 1 , wherein said labeling mixture has a pH of 7.5-8.5.

15. The method of claim 1 , wherein said labeling mixture has a pH of 8.0±0.25.

16. The method of claim 1 , wherein said labeling mixture has a pH of 8.0.

17. The method of claim 1 , further comprising analyzing said fluorescent, mass spectrometry-active derivative of said N-glycan, amine-containing amino acid, amine-containing peptide, amine-containing protein, glycosylamine, or other amine-containing compound by subjecting said fluorescent, mass spectrometry-active derivative of N-glycan, amine-containing amino acid, amine-containing peptide, amine-containing protein, glycosylamine, or other amine-containing compound to an analytical method.

18. The method of claim 17 , wherein said analytical method is selected from the group consisting of high-pressure liquid chromatography, capillary electrophoresis, fluorescence analysis, mass spectrometry, and a combination of any of these.

19. The method of claim 18 , wherein said combination is of fluorescence analysis and mass spectrometry.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 24, 2023
From: KIMZEY, MICHAEL J., DR.; GYENES, ALEXANDER, DR.
To: PROZYME, INC.
Reel/Frame 062473/0653 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 17, 2022
From: KIMZEY, MICHAEL J., DR.; GYENES, ALEXANDER, DR.
To: AGILENT TECHNOLOGIES, INC.
Reel/Frame 061443/0009 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 17, 2022
From: PROZYME, INC.
To: AGILENT TECHNOLOGIES, INC.
Reel/Frame 061443/0115 →
Continuity (3)
Continuation 15575355
Provisional Application 62168654 · May 29, 2015
Related Publication 20210223253A1 · Jul 22, 2021
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