Identification and determination of ergot alkaloids in Morning Glory cultivars

• Published in: Analytical and bioanalytical chemistry 2016-05, Vol.408 (12), p.3093-3102
• Main Authors: Nowak, Julia, Woźniakiewicz, Michał, Klepacki, Piotr, Sowa, Anna, Kościelniak, Paweł
• Format: Article
• Language: English
• Subjects: Alkaloids; Analytical Chemistry; Biochemistry; Characterization and Evaluation of Materials; Chemical properties; Chemistry; Chemistry and Materials Science; Chromatography - methods; Cultivars; Design analysis; Design optimization; Ergot alkaloids; Ergot Alkaloids - analysis; Experimental design; Extraction; Food Science; Fungi; Identification; Identification and classification; Ipomoea - chemistry; Laboratory Medicine; Limit of Detection; Liquid chromatography; LSD; Lysergic acid diethylamide; Mass spectrometry; Mass Spectrometry - methods; Mathematical analysis; Methods; Monitoring/Environmental Analysis; Morning; Psychotropic drugs; Relative abundance; Reproducibility; Reproducibility of Results; Research Paper; Seeds; Time-of-flight mass spectrometry; Ultrasonic imaging
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-016-9322-5

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. Graphical Abstract Identification of six ergot alkaloids and determination of ergine and ergometrine in Morning glory seeds using the ultrasound-assisted extraction followed the LC-MS analysis