Characterization and screening of pyrrolizidine alkaloids and N-oxides from botanicals and dietary supplements using UHPLC-high resolution mass spectrometry

Bharathi Avula; Satyanarayanaraju Sagi; Yan-Hong Wang; Jerry Zweigenbaum; Mei Wang; Ikhlas A Khan

doi:10.1016/j.foodchem.2015.01.053

Characterization and screening of pyrrolizidine alkaloids and N-oxides from botanicals and dietary supplements using UHPLC-high resolution mass spectrometry

Food Chem. 2015 Jul 1:178:136-48. doi: 10.1016/j.foodchem.2015.01.053. Epub 2015 Jan 14.

Authors

Bharathi Avula¹, Satyanarayanaraju Sagi¹, Yan-Hong Wang¹, Jerry Zweigenbaum², Mei Wang¹, Ikhlas A Khan³

Affiliations

¹ National Center for Natural Products Research, Research Institute of Pharmaceutical Sciences, The University of Mississippi, University, MS 38677, USA.
² Agilent Technologies, 2850 Centerville Rd, Wilmington, DE 19808-1610, USA.
³ National Center for Natural Products Research, Research Institute of Pharmaceutical Sciences, The University of Mississippi, University, MS 38677, USA; Division of Pharmacognosy, Department of BioMolecular Sciences, School of Pharmacy, The University of Mississippi, University, MS 38677, USA; Department of Pharmacognosy, College of Pharmacy, King Saud University, Riyadh, Saudi Arabia. Electronic address: ikhan@olemiss.edu.

PMID: 25704694
DOI: 10.1016/j.foodchem.2015.01.053

Abstract

The UHPLC-QToF-MS analysis of pyrrolizidine alkaloids (PAs) from various parts of 37 botanicals and 7 products was performed. A separation by LC was achieved using a reversed-phase column and a gradient of water/acetonitrile each containing formic acid as the mobile phase. MS-MS detection was used because of its high selectivity, and ability to provide structural information. Free base and N-oxides were observed by this method. PAs were analyzed and detected in plants from three different families, viz., Asteraceae, Boraginaceae and Fabaceae. The Asteraceae family was found to contain senecionine and lycopsamine type PAs. The Boraginaceae family contained lycopsamine and heliotrine type PAs and the Fabaceae family contained senecionine and monocrotaline type PAs. These PAs may serve as important markers for the detection of these plant materials in food and dietary supplements. PAs were identified in 44 samples by comparing their retention times, accurate mass and mass fragmentation patterns with those of 25 reference standards.

Keywords: Botanicals; Characterization; Dietary supplements; LC–QToF-MS; N-oxides; Pyrrolizidine alkaloids.

Publication types

Research Support, U.S. Gov't, Non-P.H.S.
Research Support, U.S. Gov't, P.H.S.

MeSH terms

Chromatography, High Pressure Liquid / methods*
Dietary Supplements / analysis*
Oxides / analysis
Plant Extracts / analysis*
Pyrrolizidine Alkaloids / analysis*
Tandem Mass Spectrometry / methods*

Substances

Oxides
Plant Extracts
Pyrrolizidine Alkaloids