Nowak Julia, Woźniakiewicz Michał, Klepacki Piotr, Sowa Anna, Kościelniak Paweł
Laboratory for Forensic Chemistry, Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University in Kraków, Ingardena 3, 30-060, Kraków, Poland.
Institute of Botany, Faculty of Biology and Earth Sciences, Jagiellonian University in Kraków, Kopernika 27, 31-501, Krakow, Poland.
Anal Bioanal Chem. 2016 May;408(12):3093-102. doi: 10.1007/s00216-016-9322-5. Epub 2016 Feb 12.
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.
甘薯属植物的种子含有多种麦角生物碱，包括具有精神活性的麦角酰胺和麦角新碱，常被滥用为所谓的“合法兴奋剂”。在这项工作中，开发、优化并验证了一种测定麦角酰胺和麦角新碱以及鉴定其他生物碱的分析方法。评估了三种提取技术，即浴式超声辅助提取、超声探头辅助提取和微波辅助提取，得出超声浴是提取麦角生物碱最合适的技术这一结论。随后使用Doehlert实验设计和响应面方法对提取方法进行了优化，并与优化后的液相色谱-四极杆-飞行时间质谱法一起使用。该分析程序在回收率和基质效应、重复性和中间精密度方面得到了验证。检测限和定量限分别为1.0和3.0 ng mL(-1)，足以测定甘薯种子中的麦角生物碱。分析表明，从不同供应商购买的五种种子中，只有三种含有麦角生物碱。在代表整个种子包装的样品中，生物碱的浓度及其相对丰度相似；然而，当分析单个种子时，检测到麦角酰胺和麦角新碱浓度存在显著差异。
