A liquid chromatography-electrospray ionization-mass spectrometry method for quantification of cyclotides in plants avoiding sorption during sample preparation

J Chromatogr A. 2011 Nov 4;1218(44):7964-70. doi: 10.1016/j.chroma.2011.08.095. Epub 2011 Sep 8.

Abstract

Cyclotides are plant-produced, bioactive, cyclic mini-proteins with interesting pharmaceutical and agricultural applications. A reverse phase liquid chromatography electrospray ionization mass spectrometry (RP-LC-ESI-MS) method for analysis of cyclotides in plant materials with a minimum of sample pre-treatment is presented. Three exemplary cyclotides (kalata B1, kalata B2 and cycloviolacin O2) were used as reference substances for the method development. Linearity (r(2)>0.99) was achieved in the concentration range 0.05-10 mg/L and the limit of detection was 1.7-4.0 μg/L. The present study is the first to demonstrate that cyclotides dissolved in water sorb to glass vials, but the addition of 15% of acetonitrile or 40 mg/L of bovine serum albumin is sufficient to keep the cyclotides in solution. Cyclotides were extracted from candied violets, violet tea, and the plants Oldenlandia affinis and Viola odorata using 70% methanol containing 0.1% formic acid (v/v). The plant content was determined to be 23.5-14,200 μg/g (dry weight). The highest content of cyclotide was found in wild Danish V. odorata, and it is the highest content of cyclotide in a plant reported hitherto. Candied violets contained 0.00-8.66 μg/g (dry weight), while no cyclotides were detected in commercial violet tea.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Adsorption
  • Amino Acid Sequence
  • Animals
  • Cattle
  • Chromatography, Reverse-Phase / methods*
  • Cyclotides / analysis*
  • Cyclotides / isolation & purification
  • Liquid-Liquid Extraction
  • Models, Molecular
  • Molecular Sequence Data
  • Oldenlandia / chemistry
  • Plant Extracts / chemistry*
  • Plant Proteins / analysis*
  • Plant Proteins / isolation & purification
  • Reproducibility of Results
  • Sensitivity and Specificity
  • Sequence Alignment
  • Serum Albumin, Bovine / chemistry
  • Spectrometry, Mass, Electrospray Ionization / methods*
  • Viola / chemistry

Substances

  • Cyclotides
  • Plant Extracts
  • Plant Proteins
  • Serum Albumin, Bovine