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Different Matrices for PK and Immunogenicity Assays

  • 1.  Different Matrices for PK and Immunogenicity Assays

    Community Leadership
    Posted 06-11-2025 16:32
    The use of LC/MS for the quantitation of "large molecules" such as antibodies, proteins, peptides, and antibody drug conjugates is gaining popularity.  The typical matrix for such assays is plasma.  Assessment of immunogenicity is generally required during clinical development for these modalities.  Anti-drug antibody and neutralizing antibody assays are historically ligand-binding based and utilize serum as a matrix.
     
    As part of the validation of the immunogenicity assays, the drug tolerance of the assay needs to be determined.  The results of the quantitative assays being used for pharmacokinetic assessment are then compared with the drug tolerance of immunogenicity assays to ensure that the immunogenicity results of the collected samples are not influenced by the presence of drug.  
     
    Is it a concern if the drug level assay and immunogenicity assays are run in different matrices (i.e. plasma for PK and serum for immunogenicity)?
     
    For small molecules, there are documented cases where serum levels are different from plasma levels.  These may be due, for example, to differences in stability between the matrices or cation binding of analytes impacting distribution into red blood cells, which may be disturbed when EDTA is used as the anticoagulant.
     
    Are there similar issues with "large molecules"?  While using the same matrix for both quantitative and immunogenicity assays is the "ideal" solution, in the case of ongoing programs where the two different matrices are being used, what assessments are recommended to bridge the plasma results to serum to ensure that immunogenicity results are not assessed against an inaccurate drug concentration in the sample? 
     
     


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    Eric Woolf, Ph.D., FAAPS
    Souderton, PA

    Disclaimer: Opinions expressed are solely my own and do not express the views or opinions of my employer.
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  • 2.  RE: Different Matrices for PK and Immunogenicity Assays

    Posted 06-12-2025 11:41
    Interesting question, Eric. I believe the choice of matrix often tends to be based on historical factors without a lot of scientific reasoning. For LBAs, the matrix of choice is serum more often than not, both for Pk and ADA. We should try to harmonize factors like this as much as possible.

    But you asked about ongoing programs that are using different matrices. At least for LBAs and hybrid methods, my sense is that it is not likely to make a significant difference. (Of course, then we're left with deciding what constitutes a significant difference). But keep in mind that drug tolerance is not a solidly quantitative concept. 1) drug tolerance is determined using a surrogate positive control antibody and does not necessarily reflect the behavior of patient antibodies, and 2) drug tolerance changes depending on the concentration of antibody being detected, so it's a sort of "sliding scale'.

    For these reasons I would not recommend doing any special testing to bridge the two matrices unless you have some scientific justification to think they may be different enough to impact the results of a non-quantitative ADA assay.





  • 3.  RE: Different Matrices for PK and Immunogenicity Assays

    Posted 06-13-2025 09:30
    I agree with John's response.  Unless your mAb binds to a component of the clot, which I've seen happen, then plasma and matrix should be the same for LBA.  And drug tolerance is indeed a sliding scale, it uses a surrogate of usually high affinity and there is no simple "molar ratio" determination that can readily be applied across the various combinations you could run across in real samples.






  • 4.  RE: Different Matrices for PK and Immunogenicity Assays

    Posted 06-23-2025 11:11

    To add to Eric and John's comments -

    In addition, the "drug tolerance level" is assigned based on the nominal amount of drug spiked into the validation sample, not the recovered amount that would be detected in the presence of surrogate, whereas in the study sample you'd be measuring the recovered amount of drug. It's very likely that any ADA is present in the study sample will be interfering with the PK assay measurement and probably causing under-recovery.     



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    Bonnie Rup
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  • 5.  RE: Different Matrices for PK and Immunogenicity Assays

    Past President
    Posted 06-12-2025 12:45

    Quick answer - serum is the preferred matrix for LBAs in general.  This is because it is more cleaner matrix.



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    Binodh DeSilva Ph.D.
    Senior Vice President
    Ultragenyx
    Skillman NJ
    [email protected]

    Disclaimer: Opinions expressed are solely my own and do not express the views or opinions of my employer.
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  • 6.  RE: Different Matrices for PK and Immunogenicity Assays

    Community Leadership
    Posted 07-21-2025 13:07

    I think that plasma may now be an acceptable choice for both PK and ADA assays in the context that our assays are getting much better at dealing with interference. We can even use whole blood microsamples. It's also a little easier on the clinical sites to collect plasma since it can be spun immediately after collection. So I wouldn't necessarily say that you have to use different matrices even if you feel that you need to use plasma for PK

    If this is a legacy decision, you can always qualify the PK assay in serum and run some selected ADA samples to see if there is a correction factor needed. 



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    Joleen White Ph.D.
    AAPS 2024 Global Health Community Chair
    Bioanalytical 101 Course Development
    Senior Advisor
    BioData Solutions LLC
    [email protected]

    Disclaimer: Opinions expressed are solely my own and do not express the views or opinions of my employer.
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  • 7.  RE: Different Matrices for PK and Immunogenicity Assays

    Posted 07-21-2025 14:06
    For run-of-the-mill mAb or pAb (like ADA), serum or plasma should be much the same for PK/ADA.  If you have a drug that somehow gets sequestered in a clot component for whatever reason, then serum won't be a good matrix.  Plasma has an issue operationally as sometimes it can clot in an assay plate or even sample tubes (though not if you're careful about it).  Another consideration:  If you might use PK/ADA samples for subsequent biomarker analysis, or want to use one collection tube type for all these BA samples, and your biomarker exists in platelets (many do), then plasma might be the better choice.





  • 8.  RE: Different Matrices for PK and Immunogenicity Assays

    Posted 07-22-2025 13:35

    Plasma is a problematic matrix for platforms with microcapillaries (e.g. Gyros).  Sampling needles get frequently clogged as well with plasma 'stuff.' 

    If you have a choice, choose serum as your matrix.

     

    Uma Kavita, Ph.D.

    Senior Director, Oncology Integrated Bioanalysis Strategy

    AstraZeneca

    R&D | Clinical Pharmacology & Safety Sciences

     


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  • 9.  RE: Different Matrices for PK and Immunogenicity Assays

    Community Leadership
    Posted 06-13-2025 10:01

    I am less concerned about mAbs.  What do people think regarding the smaller peptides (some cyclic) that are under development by several companies?   



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    Eric Woolf, Ph.D., FAAPS
    Souderton, PA

    Disclaimer: Opinions expressed are solely my own and do not express the views or opinions of my employer.
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  • 10.  RE: Different Matrices for PK and Immunogenicity Assays

    Community Leadership
    Posted 06-13-2025 10:03

    For small peptides, can RBC binding be impacted by anticoagulants?  Can stability in serum be different from that in plasma?



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    Eric Woolf, Ph.D., FAAPS
    Souderton, PA

    Disclaimer: Opinions expressed are solely my own and do not express the views or opinions of my employer.
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  • 11.  RE: Different Matrices for PK and Immunogenicity Assays

    Posted 06-16-2025 13:27

    If your drug binds to or even, goes into the blood cells I would expect difference in the concentrations measured in serum vs. plasma. For example, I used to see 10x concentration difference of the brain factor BDNF in serum vs. plasma, because of this, BDNF is tested in platelet poor plasma samples. For the question about stability, I saw difference for a functional assay, which probably due to that the enzyme activity relies on cofactors in the matrix, but we didn't see stability difference in the correlated protein (PK) assay. 



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    Rachel Wang, Ph.D.
    Bioanalytical assay development lead
    Spark Therapeutics
    Philadelphia, PA.
    [email protected]

    Disclaimer: Opinions expressed are solely my own and do not express the views or opinions of my employer.
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