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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
Food chemistry 2015 v.178 pp. 136-148
Ageratum, Borago, Crotalaria, Eupatorium, Heliotropium, Petasites, Senecio, Symphytum, Tussilago, acetonitrile, detection, dietary supplements, food composition, formic acid, mass spectrometry, methanol, monocrotaline, nitrogen oxides, plant extracts, reference standards, screening
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.