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Title: Characterization and screening of pyrrolizidine alkaloids and N-oxides from various parts of many botanicals and dietary supplements using liquid chromatography high resolution mass spectrometry

Author
item AVULA, BHARATHI - University Of Mississippi
item SAGI, SATYANARAYANARA - University Of Mississippi
item WANG, YAN-HONG - University Of Mississippi
item ZWEIGENBAUM, JERRY - University Of Mississippi
item WANG, MEI - University Of Mississippi
item KHAN, IKHLAS - University Of Mississippi

Submitted to: Food Chemistry
Publication Type: Peer Reviewed Journal
Publication Acceptance Date: 1/8/2015
Publication Date: 1/14/2015
Publication URL: http://handle.nal.usda.gov/10113/62344
Citation: Avula, B., Sagi, S.J., Wang, Y., Zweigenbaum, J., Wang, M., Khan, I.A. 2015. Characterization and screening of pyrrolizidine alkaloids and N-oxides from various parts of many botanicals and dietary supplements using liquid chromatography high resolution mass spectrometry. Food Chemistry. 178:136-148.

Interpretive Summary: Botanicals used in dietary supplements should be devoid of Pyrrolizidine Alkaloids s which cause liver toxicity. The combination of LC and QToF-mass spectrometry provided a rapid screening of pyrrolizidine alkaloids from plant samples and dietary supplements. The method developed was sensitive and provided an effective approach for characterization of Pyrrolizidine Alkaloids bases/N-oxides from botanicals and dietary supplements in a single chromatographic run. The Pyrrolizidine Alkaloids, intermedine and lycopsamine were detected in many species of Borago, Symphytum, Crotalaria and Eupatorium. Out of 7 dietary supplements analyzed, 5 showed for the presence of Pyrrolizidine Alkaloids.

Technical Abstract: The UHPLC-QToF-MS analysis of pyrrolizidine alkaloids from various parts of 37 botanicals and 7 dietary supplements 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, sensitivity and ability to provide structural information. Free base and N-oxide derivatives were observed by this method. The extraction of botanicals was investigated by various procedures including: (a) sonication with methanol, (b) sonication with acidified aqueous methanol, (c) alkaloidal extraction, and (d) microwave extraction with acidified aqueous methanol. pyrrolizidine alkaloids were analyzed and detected in plants from three different families, Viz., Asteraceae (Senecio spp., Eupatorium spp., Ageratum spp., Tussilago spp., Petasites spp.,), Boraginaceae (Heliotropium spp., Symphytum spp., Borago spp.), and Fabaceae (Crotalaria spp.). The Astraceae family was found to contain senecionine and lycopsamine type pyrrolizidine alkaloids. The Boraginaceae family contained lycopsamine and heliotrine type pyrrolizidine alkaloids and the Fabaceae family contained senecionine and monocrotaline type pyrrolizidine alkaloids. These pyrrolizidine alkaloids may serve as important markers for the detection of these plant materials in food and dietary supplements. pyrrolizidine alkaloids were identified in 44 samples (botanicals and dietary supplements) by comparing their retention times, accurate mass and mass fragmentation patterns with those of 25 reference standards.