Rapid quantification of a cleavable antibody-conjugated drug by liquid chromatography/tandem mass spectrometry with microwave-assisted enzymatic cleavage

J Pharm Biomed Anal. 2016 Sep 5:128:226-235. doi: 10.1016/j.jpba.2016.05.043. Epub 2016 May 24.

Abstract

Antibody-drug conjugates (ADCs) play an increasingly important role for targeted cancer treatment. One class of ADCs has attracted particular interest in drug development. These ADCs employ a cleavable chemistry linkage for drugs and utilize the reduced interchain disulfide cysteine residues for conjugation. In this work, a novel bioanalytical method for the quantification of a cleavable antibody-conjugated drug in plasma was developed, qualified, and implemented. This novel method significantly improves throughput by combining a microwave-assisted, enzymatic cleavage of conjugated drugs from ADCs with a 96-well based sample preparation procedure to immunocapture ADCs in plasma. The released drug is subsequently quantified using a LC/MS/MS method. Our results represent a high-throughput, generic, and sensitive quantification method for antibody-conjugated microtubule inhibitors (such as MMAE) for preclinical PK/PD studies. The linear range of the standard curve for antibody conjugated drug (MMAE) was from 2.01 to 2010ng/mL with an excellent linearity (r(2)>0.997). The intra-run precision was below 8.14% and accuracy was from -7.71% to -1.08%. No matrix effect or carryover was observed for this method. This method was successfully used to measure the level of conjugated drug in a preclinical PK/PD study in mice.

Keywords: Antibody-conjugated drug; Drug antibody ratio; Immunocapture mass spectrometry; MMAE; Microwave-assisted hydrolysis.

MeSH terms

  • Animals
  • Azides / chemistry
  • Biotin / chemistry
  • Cathepsin B / chemistry
  • Chromatography, High Pressure Liquid
  • Enzymes / chemistry
  • Female
  • Hydrolysis
  • Immunoconjugates / analysis*
  • Immunoconjugates / pharmacokinetics*
  • Mice
  • Mice, SCID
  • Microtubule Proteins / antagonists & inhibitors
  • Microwaves
  • Oligopeptides / chemistry
  • Propanolamines / chemistry
  • Quality Control
  • Reproducibility of Results
  • Tandem Mass Spectrometry

Substances

  • Azides
  • Enzymes
  • Immunoconjugates
  • Microtubule Proteins
  • Oligopeptides
  • Propanolamines
  • Biotin
  • 4-azidobenzylcarazolol
  • Cathepsin B
  • monomethyl auristatin E