Synthesis and NMR Characterization of the Prenylated Peptide, a-Factor

Methods Enzymol. 2019:614:207-238. doi: 10.1016/bs.mie.2018.09.025. Epub 2018 Dec 22.

Abstract

Protein and peptide prenylation is an essential biological process involved in many signal transduction pathways. Hence, it plays a critical role in establishing many major human ailments, including Alzheimer's disease, amyotrophic lateral sclerosis (ALS), malaria, and Ras-related cancers. Yeast mating pheromone a-factor is a small dodecameric peptide that undergoes prenylation and subsequent processing in a manner identical to larger proteins. Due to its small size in addition to its well-characterized behavior in yeast, a-factor is an attractive model system to study the prenylation pathway. Traditionally, chemical synthesis and characterization of a-factor have been challenging, which has limited its use in prenylation studies. In this chapter, a robust method for the synthesis of a-factor is presented along with a description of the characterization of the peptide using MALDI and NMR. Finally, complete assignments of resonances from the isoprenoid moiety and a-factor from COSY, TOCSY, HSQC, and long-range HMBC NMR spectra are presented. This methodology should be useful for the synthesis and characterization of other mature prenylated peptides and proteins.

Keywords: C-terminal ester; Farnesylation; Lipidation; NMR; Peptide; Pheromone; Prenylation; a-Factor.

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.

MeSH terms

  • Chromatography, Affinity / methods
  • Fluorenes / chemistry*
  • Humans
  • Mating Factor / chemical synthesis
  • Mating Factor / chemistry*
  • Mating Factor / isolation & purification
  • Nuclear Magnetic Resonance, Biomolecular / methods*
  • Peptides / chemical synthesis
  • Peptides / chemistry*
  • Peptides / isolation & purification
  • Protein Prenylation
  • Saccharomyces cerevisiae / chemistry*
  • Saccharomyces cerevisiae / metabolism
  • Solid-Phase Synthesis Techniques / methods*
  • Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization / methods
  • Trityl Compounds / chemistry

Substances

  • Fluorenes
  • Peptides
  • Triphenylmethyl Compounds
  • alpha-factor (Saccharomyces cerevisiae)
  • Mating Factor
  • trityl chloride