IP Library › Granted Patent US 12,517,024
Granted Patent B2
US 12,517,024 · App. 17/869,194 · Granted Jan 6, 2026

Method of evaluating the enamel microcrack resistance efficacy of compositions

Inventors: Qichao Ruan (Hillsborough, NJ); Stacey Lavender (Chesterfield, NJ)
Assignee: Colgate-Palmolive Company
G01N3/46A61K6/20
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Quick Facts
Patent No.
US 12,517,024
App. No.
17/869,194
Granted
Jan 6, 2026
Kind
B2
Abstract

Disclosed are methods of determining enamel micro-crack and/or microscratch resistance and also methods of identifying compositions that are effective in increasing enamel micro-crack and/or microscratch resistance or evaluating the efficacy of compositions in increasing enamel micro-crack and/or microscratch resistance.

Claims (33)

1 . A method of identifying compositions that are effective in increasing enamel micro-crack resistance or evaluating the efficacy of compositions in increasing enamel micro-crack resistance; comprising:

a) providing an enamel sample;

b) generating baseline micro-cracks on the enamel sample;

c) measuring and/or calculating one or more baseline micro-crack characteristics or mechanical properties of the enamel;

d) treating the enamel sample with a composition;

e) generating post-treatment micro-cracks on the enamel sample;

f) measuring and/or calculating one or more post-treatment micro-crack characteristics or mechanical properties of the enamel;

g) determining one or more parameters which are changes of the one or more micro-crack characteristics or mechanical properties of the enamel by calculating the difference between the corresponding values obtained before and after the treatment;

h) comparing the one or more parameters of the composition with those of a control composition; and

i) selecting or identifying the composition for further development or evaluating the efficacy of the composition in increasing enamel micro-crack resistance based on its ability to increase micro-crack resistance relative to the control composition.

2 . The method of claim 1 , wherein the micro-cracks are generated by impressing an indenter into the enamel sample with a load.

3 . The method of claim 1 , wherein the enamel sample is a human or bovine enamel.

4 . The method of claim 2 , wherein the load is 200 gf-1000 gf.

5 . The method of claim 1 , wherein in steps c) and f), the one or more micro-crack characteristics or mechanical properties of the enamel are selected from crack length, fracture toughness, brittleness, and a combination thereof.

6 . The method of claim 1 , wherein the composition is an oral care composition.

7 . The method of claim 1 , wherein the one or more parameters is selected from change in crack length, change in fracture toughness, change in brittleness and a combination thereof.

8 . A method of identifying compositions that are effective in increasing enamel microscratch resistance or evaluating the efficacy of compositions in increasing enamel microscratch resistance; comprising:

a) providing an enamel sample;

b) generating baseline microscratches on the enamel sample;

c) measuring and/or calculating one or more baseline microscratch characteristics or mechanical properties of the enamel;

d) treating the enamel sample with a test composition;

e) generating post-treatment microscratches on the enamel sample;

f) measuring and/or calculating one or more post-treatment microscratch characteristics or mechanical properties of the enamel;

g) determining one or more parameters which are changes of the one or more microscratch characteristics or mechanical properties of the enamel by calculating the difference between the corresponding values obtained before and after the treatment;

h) comparing the one or more parameters of the composition with those of a control composition; and

i) selecting or identifying the composition for further development or evaluating the efficacy of the composition in increasing enamel microscratch resistance based on its ability to increase microscratch resistance relative to the control composition.

9 . The method of claim 8 , wherein the enamel sample is a human or bovine enamel.

10 . The method of claim 8 , wherein the microscratches are generated by nanoindentation to generate a baseline microscratch (microscratch 1).

11 . The method of claim 8 , wherein the microscratch is generated by maintaining a force from 5 mN-50 mN upon the enamel.

12 . The method of claim 8 , wherein the enamel is treated with the test composition.

13 . The method of claim 8 , wherein the enamel is subjected to an acid challenge subsequent to being treated with a test composition.

14 . The method of claim 8 , wherein the enamel samples are subject to further microscratches (microscratch 2) subsequent to treatment with the test composition and/or acid challenge.

15 . The method of claim 8 , wherein the test composition in step d) is an oral care composition, the control composition is the same type of oral care composition as the test composition, and the control composition does not contain any ingredient that affects physical properties of tooth enamel.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 30, 2025
From: RUAN, QICHAO; LAVENDER, STACEY
To: COLGATE-PALMOLIVE COMPANY
Reel/Frame 071567/0752 →
Continuity (2)
Provisional Application 63223726 · Jul 20, 2021
Related Publication 20230042124A1 · Feb 9, 2023
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