Structure-Activity Relationship of Sulfonyl Piperazine LpxH Inhibitors Analyzed by an LpxE-Coupled Malachite Green Assay

ACS Infect Dis. 2019 Apr 12;5(4):641-651. doi: 10.1021/acsinfecdis.8b00364. Epub 2019 Feb 5.

Abstract

The UDP-2,3-diacylglucosamine pyrophosphatase LpxH in the Raetz pathway of lipid A biosynthesis is an essential enzyme in the vast majority of Gram-negative pathogens and an excellent novel antibiotic target. The 32P-radioautographic thin-layer chromatography assay has been widely used for analysis of LpxH activity, but it is inconvenient for evaluation of a large number of LpxH inhibitors over an extended time period. Here, we report a coupled, nonradioactive LpxH assay that utilizes the recently discovered Aquifex aeolicus lipid A 1-phosphatase LpxE for quantitative removal of the 1-phosphate from lipid X, the product of the LpxH catalysis; the released inorganic phosphate is subsequently quantified by the colorimetric malachite green assay, allowing the monitoring of the LpxH catalysis. Using such a coupled enzymatic assay, we report the biochemical characterization of a series of sulfonyl piperazine LpxH inhibitors. Our analysis establishes a preliminary structure-activity relationship for this class of compounds and reveals a pharmacophore of two aromatic rings, two hydrophobic groups, and one hydrogen-bond acceptor. We expect that our findings will facilitate the development of more effective LpxH inhibitors as potential antibacterial agents.

Keywords: Gram-negative bacteria; LpxE; LpxH; enzyme-coupled assay; lipid A; novel antibiotics.

Publication types

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

MeSH terms

  • Anti-Bacterial Agents / chemistry
  • Anti-Bacterial Agents / pharmacology
  • Aquifex
  • Bacteria / chemistry
  • Bacteria / enzymology*
  • Bacterial Proteins / antagonists & inhibitors
  • Bacterial Proteins / chemistry*
  • Biocatalysis
  • Enzyme Assays
  • Enzyme Inhibitors / chemistry*
  • Enzyme Inhibitors / pharmacology
  • Escherichia coli / chemistry
  • Escherichia coli / drug effects
  • Escherichia coli / enzymology*
  • Escherichia coli / genetics
  • Glycolipids / chemistry
  • Phosphates / chemistry*
  • Piperazine / chemistry*
  • Piperazine / pharmacology
  • Pyrophosphatases / antagonists & inhibitors
  • Pyrophosphatases / chemistry*
  • Rosaniline Dyes / chemistry*
  • Structure-Activity Relationship

Substances

  • Anti-Bacterial Agents
  • Bacterial Proteins
  • Enzyme Inhibitors
  • Glycolipids
  • Phosphates
  • Rosaniline Dyes
  • malachite green
  • Piperazine
  • lipid X
  • Pyrophosphatases
  • UDP-2,3-diacylglucosamine pyrophosphatase

Supplementary concepts

  • Aquifex aeolicus