An efficient and inexpensive refrigerated LC system for H/D exchange mass spectrometry

J Am Soc Mass Spectrom. 2011 Aug;22(8):1472-6. doi: 10.1007/s13361-011-0152-6. Epub 2011 May 15.

Abstract

Loss of deuterium label during the LC step in amide hydrogen/deuterium exchange mass spectrometry (H/D-MS) is minimized by maintaining an acidic mobile phase pH and low temperature (pH 2.5, 0 °C). Here we detail the construction and performance of a low-cost, thermoelectrically refrigerated enclosure to house high-performance liquid chromatography (HPLC) components and cool mobile phases. Small volume heat exchangers rapidly decrease mobile phase temperature and keep the temperature stable to ±0.2 °C. Using a superficially porous reversed-phase column, we obtained excellent chromatographic performance in the separation of peptides with a median peak width of 4.4 s. Average deuterium recovery was 80.2% with an average relative precision of 0.91%.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Amino Acid Sequence
  • Chromatography, High Pressure Liquid
  • Chromatography, Reverse-Phase / instrumentation
  • Chromatography, Reverse-Phase / methods*
  • Deuterium Exchange Measurement / methods*
  • Equipment Design
  • Hydrogen-Ion Concentration
  • Mass Spectrometry / methods*
  • Molecular Sequence Data
  • Peptides / chemistry
  • Refrigeration / instrumentation*
  • Temperature

Substances

  • Peptides