Fluorescence labeling, purification, and immobilization of a double cysteine mutant calmodulin fusion protein for single-molecule experiments

Anal Biochem. 2004 Feb 15;325(2):273-84. doi: 10.1016/j.ab.2003.10.045.

Abstract

We present a method of labeling and immobilizing a low-molecular-weight protein, calmodulin (CaM), by fusion to a larger protein, maltose binding protein (MBP), for single-molecule fluorescence experiments. Immobilization in an agarose gel matrix eliminates potential interactions of the protein and the fluorophore(s) with a glass surface and allows prolonged monitoring of protein dynamics. The small size of CaM hinders its immobilization in low-weight-percentage agarose gels; however, fusion of CaM to MBP via a flexible linker provides sufficient restriction of translational mobility in 1% agarose gels. Cysteine residues were engineered into MBP.CaM (MBP-T34C,T110C-CaM) and labeled with donor and acceptor fluorescent probes yielding a construct (MBP.CaM-DA) which can be used for single-molecule single-pair fluorescence resonance energy transfer (spFRET) experiments. Mass spectrometry was used to verify the mass of MBP.CaM-DA. Assays measuring the activity of CaM reveal minimal activity differences between wild-type CaM and MBP.CaM-DA. Single-molecule fluorescence images of the donor and acceptor dyes were fit to a two-dimensional Gaussian function to demonstrate colocalization of donor and acceptor dyes. FRET is demonstrated both in bulk fluorescence spectra and in fluorescence trajectories of single MBP.CaM-DA molecules. The extension of this method to other biomolecules is also proposed.

Publication types

  • Research Support, N.I.H., Extramural
  • Research Support, Non-U.S. Gov't
  • Research Support, U.S. Gov't, Non-P.H.S.
  • Research Support, U.S. Gov't, P.H.S.

MeSH terms

  • Calmodulin / chemistry*
  • Calmodulin / genetics
  • Calmodulin / isolation & purification
  • Carrier Proteins / chemistry*
  • Carrier Proteins / genetics
  • Carrier Proteins / isolation & purification
  • Cysteine / chemistry*
  • Cysteine / genetics
  • Maltose-Binding Proteins
  • Mass Spectrometry
  • Mutation
  • Recombinant Fusion Proteins / chemistry*
  • Recombinant Fusion Proteins / genetics
  • Recombinant Fusion Proteins / isolation & purification
  • Spectrometry, Fluorescence
  • Succinimides
  • Xanthenes

Substances

  • Alexa Fluor 488 carboxylic acid succinimidyl ester
  • Calmodulin
  • Carrier Proteins
  • Maltose-Binding Proteins
  • Recombinant Fusion Proteins
  • Succinimides
  • Xanthenes
  • Texas red
  • Cysteine