IP Library Granted Patent US 12710364
Granted Patent B2
US 12710364 · App. 17/928,671 · Granted Aug 18, 2026

Assessment of cleaning procedures of a biotherapeutic manufacturing process

Inventor: Rammahipal Kouda (Thousand Oaks, CA)
Assignee: AMGEN INC.
G01N21/554G01N21/94G01N30/02G01N33/54366G01N2030/027
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Quick Facts
Patent No.
US 12710364
App. No.
17/928,671
Granted
Aug 18, 2026
Kind
B2
Abstract

Provided herein are methods of assessing or validating a cleaning procedure of a biotherapeutic manufacturing process, said method comprising analyzing by a surface plasmon resonance (SPR)-based assay the binding activity of a cleaned sample to a ligand which binds to a biotherapeutic produced by the manufacturing process. In various embodiments, the cleaning procedure comprises one or more steps to inactivate and/or degrade the biotherapeutic. In various instances, the method demonstrates that greater than about 99.99% degradation of the therapeutic is achieved by the cleaning procedure comprising the one or more steps to inactivate and/or degrade the biotherapeutic.

Claims (28)

1 . A cleaning validation assay for a biotherapeutic manufacturing process, comprising: determining the binding activity of a cleaned sample to a ligand by a surface plasmon resonance (SPR)-based assay, where in the which binds to the biotherapeutic produced by the biotherapeutic manufacturing process wherein the cleaned sample is obtained by carrying out a small-scale cleaning procedure, which simulates a large-scale cleaning procedure, on a sample comprising the biotherapeutic, wherein the cleaning validation assay has a limit of detection (LOD) that is less than 20 ng/mL.

2 . The cleaning validation assay of claim 1 , wherein the biotherapeutic comprises an Fc domain and/or the ligand is an Fc-binding protein.

3 . The cleaning validation assay of claim 2 , wherein the biotherapeutic is an antibody.

4 . The cleaning validation assay of claim 2 , wherein the Fc-binding protein is Protein A, Protein G, or Protein L.

5 . The cleaning validation assay of claim 2 , wherein the biotherapeutic is a bispecific T-cell engager molecule comprising a CD3-binding domain.

6 . The cleaning validation assay of claim 5 , wherein the ligand comprises a CD3 epitope that binds to the CD3-binding domain.

7 . The cleaning validation assay of claim 1 , wherein the acceptable daily exposure (ADE) of the biotherapeutic is 0.1 μg to 1 μg.

8 . A method of assessing a cleaning procedure of a biotherapeutic manufacturing process, comprising:

a. carrying out a small-scale cleaning procedure, which simulates a large-scale cleaning procedure, on a sample comprising the biotherapeutic produced by the biotherapeutic manufacturing process, to obtain a cleaned sample,

b. determining the binding activity of the cleaned sample to a ligand which binds to the biotherapeutic, wherein the binding activity is determined by a surface plasmon resonance (SPR)-based assay, which correlates the binding activity to a concentration of the biotherapeutic; and

c. determining the concentration of the biotherapeutic of the cleaned sample based on the binding activity determined by the SPR-based assay.

9 . The method of claim 8 , wherein the cleaning procedure comprises at least one degradation step and/or at least one inactivation step purposed for degrading and/or inactivating the biotherapeutic.

10 . The method of claim 9 , which demonstrates greater than about 99.99% degradation of the biotherapeutic.

11 . The method of claim 10 , which demonstrates greater than about 99.999% degradation of the biotherapeutic.

12 . The method of claim 8 , wherein the cleaning procedure comprises an alkaline wash, an acidic wash, a high temperature step, or any combination thereof.

13 . The method of claim 8 , wherein the cleaned sample is filtered through a filter before determining the binding activity or the method comprises filtering the cleaned sample through a filter to reduce the amount of precipitates or salt crystals in the cleaned sample and/or to reduce the overall volume of the cleaned sample, optionally, wherein the filtering increases a protein concentration of the cleaned sample.

14 . The method of claim 13 , comprising filtering the cleaned sample through a PES filter and/or a MWCO filter having a MWCO of about 30 kDa to about 50 kDa.

15 . The method of claim 8 , wherein the ligand is attached to a face of a solid support.

16 . The method of claim 8 , wherein the binding activity correlates with a concentration of an active form of the biotherapeutic in the solution.

17 . The method of claim 16 , further comprising comparing the change in the SPR angle to a calibration curve to obtain a concentration of the active form of the biotherapeutic in the solution.

18 . The method of claim 8 , wherein the biotherapeutic comprises an Fc domain and/or the ligand is an Fc-binding protein.

19 . The method of claim 18 , wherein the biotherapeutic is an antibody.

20 . The method of claim 18 , the Fc-binding protein is Protein A, Protein G, or Protein L.

21 . The method of claim 8 , wherein the biotherapeutic is a bispecific T-cell engager molecule comprising a CD3-binding domain.

22 . The method of claim 21 , wherein the ligand comprises a CD3 epitope that binds to the CD3-binding domain.

23 . The method of claim 8 , wherein the limit of detection (LOD) for the active form of the biotherapeutic is less than about 20 ng/mL.

24 . The method of claim 8 , wherein the LOD for the active form of the biotherapeutic is about 13.0 ng/nL or less.

25 . The method of claim 8 , wherein the acceptable daily exposure (ADE) of the biotherapeutic is 0.1 μg to 1 μg.