title: Identification and determination of ergot alkaloids in Morning Glory cultivars.
abstract: Seeds of plants from Ipomoea genera contain numerous ergot alkaloids, including psychoactive ergine and ergometrine, and are often abused as so-called "legal highs." In this work, an analytical method for determination of ergine and ergometrine, and identification of other alkaloids was developed, optimized, and validated. Three extraction techniques, ultrasound-assisted extraction in bath, or with sonotrode, and microwave-assisted extraction were evaluated, and it was concluded that ultrasonic bath is the most suitable technique for extraction of ergot alkaloids. The extraction method was later optimized using a Doehlert experimental design with response surface methodology and used together with the optimized LC-Q-TOF-MS method. The analytical procedure was validated in terms of recovery and matrix effect, repeatability, and intermediate precision. Limits of detection and quantification were 1.0 and 3.0 ng mL(-1), respectively, and were sufficient for determination of ergot alkaloids in Ipomoea seeds. The analysis revealed that from five kinds of seeds purchased from different vendors, only three contained ergot alkaloids. Concentration of alkaloids and their relative abundance was similar in samples representative for whole seeds packs; however, when single seeds were analyzed, significant discrepancies in ergine and ergometrine concentrations were detected.
authors.affiliation: Laboratory for Forensic Chemistry, Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University in Kraków, Ingardena 3, 30-060, Kraków, Poland.
authors.forename: Julia
authors.initials: J
authors.lastname: Nowak
authors.affiliation: Laboratory for Forensic Chemistry, Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University in Kraków, Ingardena 3, 30-060, Kraków, Poland. michal.wozniakiewicz@uj.edu.pl.
authors.forename: Michał
authors.initials: M
authors.lastname: Woźniakiewicz
authors.affiliation: Institute of Botany, Faculty of Biology and Earth Sciences, Jagiellonian University in Kraków, Kopernika 27, 31-501, Krakow, Poland.
authors.forename: Piotr
authors.initials: P
authors.lastname: Klepacki
authors.affiliation: Laboratory for Forensic Chemistry, Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University in Kraków, Ingardena 3, 30-060, Kraków, Poland.
authors.forename: Anna
authors.initials: A
authors.lastname: Sowa
authors.affiliation: Laboratory for Forensic Chemistry, Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University in Kraków, Ingardena 3, 30-060, Kraków, Poland.
authors.forename: Paweł
authors.initials: P
authors.lastname: Kościelniak
mesh_terms: D002845:Chromatography / Q000379:methods; D004876:Ergot Alkaloids / Q000032:analysis*; D027741:Ipomoea / Q000737:chemistry*; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000379:methods; D015203:Reproducibility of Results
chemical_list: D004876:Ergot Alkaloids
keywords: Ergine; Ergometrine; Ipomoea; LC-MS; Morning Glory; UAE