title: Simultaneous separation of ergot alkaloids by capillary electrophoresis after cloud point extraction from cereal samples.
abstract: A new and sensitive analytical methodology for ergot alkaloids (EA) determination from cereal samples based on cloud point extraction (CPE) prior to CE-UV absorbance was developed. The methodology involves extraction under acid conditions and subsequent preconcentration by applying a simple, rapid and environmentally friendly low volume surfactant extraction procedure. After extraction, CE analysis was carried out by performing dilutions on preconcentrated surfactant rich phase, achieving a single peak or simultaneous alkaloids determination. A real preconcentration factor of 22 of total EA was obtained, demonstrating the efficiency of this methodology. The limits of detection were 2.6 and 2.2 μg/kg for ergotamine and ergonovine, respectively. Validation procedure revealed suitable linearity, accuracy and precision. The average extraction and clean-up recoveries were compared with the theoretical values and were better than 92%. This method was successfully applied to the determination of EA in different varieties of commercial flour samples, two grain samples and one of the leading brands cereal-based product for infant feeding. The high sensitivity achieved for EA determinations in real samples suggests CPE procedure as an interesting approach to improve CE-UV visible detection limits. Moreover, the whole process could be considered as a contribution to green chemistry because nonorganic solvents were involved, demonstrating its great potential over conventional techniques.
authors.affiliation: INQUISAL-CONICET, San Luis, Argentina.
authors.forename: Emiliano
authors.initials: E
authors.lastname: Felici
authors.forename: Chien C
authors.initials: CC
authors.lastname: Wang
authors.forename: Liliana P
authors.initials: LP
authors.lastname: Fernández
authors.forename: María R
authors.initials: MR
authors.lastname: Gomez
mesh_terms: D002523:Edible Grain / Q000737:chemistry*; D019075:Electrophoresis, Capillary / Q000379:methods*; D004876:Ergot Alkaloids / Q000032:analysis*; D005433:Flour / Q000032:analysis; D005506:Food Contamination / Q000032:analysis*; D057230:Limit of Detection; D059625:Liquid-Liquid Extraction / Q000379:methods; D015203:Reproducibility of Results; D013056:Spectrophotometry, Ultraviolet; D013501:Surface-Active Agents / Q000737:chemistry
chemical_list: D004876:Ergot Alkaloids; D013501:Surface-Active Agents
keywords: Capillary electrophoresis; Cereals; Ergot alkaloids; Ergotamine