High-resolution α-amylase assay combined with high-performance liquid chromatography-solid-phase extraction-nuclear magnetic resonance spectroscopy for expedited identification of α-amylase inhibitors: proof of concept and α-amylase inhibitor in cinnamon

J Agric Food Chem. 2014 Nov 26;62(47):11465-71. doi: 10.1021/jf5047283. Epub 2014 Nov 17.

Abstract

Type 2 diabetes affects millions of people worldwide, and new improved drugs or functional foods containing selective α-amylase inhibitors are needed for improved management of blood glucose. In this article the development of a microplate-based high-resolution α-amylase inhibition assay with direct photometric measurement of α-amylase activity is described. The inhibition assay is based on porcine pancreatic α-amylase with 2-chloro-4-nitrophenyl-α-D-maltotriose as substrate, which this gives a stable, sensitive, and cheap inhibition assay as requested for high-resolution purposes. In combination with HPLC-HRMS-SPE-NMR, this provides an analytical platform that allows simultaneous chemical and biological profiling of α-amylase inhibitors in plant extracts. Proof-of-concept with an artificial mixture of six compounds-of which three are known α-amylase inhibitors-showed that the high-resolution α-amylase inhibition profiles allowed detection of sub-microgram amounts of the α-amylase inhibitors. Furthermore, the high-resolution α-amylase inhibition assay/HPLC-HRMS-SPE-NMR platform allowed identification of cinnamaldehyde as the α-amylase inhibitor in cinnamon (Cinnamomum verum Presl.).

Keywords: HPLC−HRMS−SPE−NMR; high-resolution α-amylase assay; microplate; type 2 diabetes.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Acrolein / analogs & derivatives
  • Acrolein / analysis
  • Animals
  • Chromatography, High Pressure Liquid / methods*
  • Cinnamomum zeylanicum / chemistry*
  • Enzyme Inhibitors / analysis*
  • Magnetic Resonance Spectroscopy / methods*
  • Pancreatic alpha-Amylases / antagonists & inhibitors*
  • Plant Extracts / chemistry
  • Reproducibility of Results
  • Solid Phase Extraction / methods*
  • Swine
  • Trisaccharides / metabolism

Substances

  • Enzyme Inhibitors
  • Plant Extracts
  • Trisaccharides
  • 2-chloro-4-nitrophenylmaltotrioside
  • Acrolein
  • Pancreatic alpha-Amylases
  • cinnamaldehyde