Minimizing carry-over in an online pepsin digestion system used for the H/D exchange mass spectrometric analysis of an IgG1 monoclonal antibody

J Am Soc Mass Spectrom. 2012 Dec;23(12):2140-8. doi: 10.1007/s13361-012-0485-9. Epub 2012 Sep 20.

Abstract

Chromatographic carry-over can severely distort measurements of amide H/D exchange in proteins analyzed by LC/MS. In this work, we explored the origin of carry-over in the online digestion of an IgG1 monoclonal antibody using an immobilized pepsin column under quenched H/D exchange conditions (pH 2.5, 0 °C). From a consensus list of 169 different peptides consistently detected during digestion of this large, ~150 kDa protein, approximately 30% of the peptic peptides exhibited carry-over. The majority of carry-over originates from the online digestion. Carry-over can be substantially decreased by washing the online digestion flow-path and pepsin column with two wash cocktails: [acetonitrile (5%)/isopropanol (5%)/acetic acid (20%) in water] and [2 M guanidine hydrochloride in 100 mM phosphate buffer pH 2.5]. Extended use of this two-step washing procedure does not adversely affect the specificity or activity of the immobilized pepsin column. The results suggest that although the mechanism of carry-over appears to be chemical in nature, and not hydrodynamic, carry-over cannot be attributed to a single factor such as mass, abundance, pI, or hydrophobicity of the peptides.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Antibodies, Monoclonal / analysis*
  • Antibodies, Monoclonal / chemistry
  • Antibodies, Monoclonal / metabolism
  • Chromatography, Liquid / instrumentation
  • Chromatography, Liquid / methods
  • Deuterium Exchange Measurement / instrumentation
  • Deuterium Exchange Measurement / methods*
  • Equipment Design
  • Hydrogen-Ion Concentration
  • Immunoglobulin G / analysis*
  • Immunoglobulin G / chemistry
  • Immunoglobulin G / metabolism
  • Linear Models
  • Pepsin A / chemistry*
  • Pepsin A / metabolism
  • Peptide Fragments / analysis*
  • Peptide Fragments / chemistry
  • Peptide Fragments / metabolism
  • Reproducibility of Results
  • Spectrometry, Mass, Electrospray Ionization / instrumentation
  • Spectrometry, Mass, Electrospray Ionization / methods*
  • Temperature

Substances

  • Antibodies, Monoclonal
  • Immunoglobulin G
  • Peptide Fragments
  • Pepsin A