Development and validation of an analytical method for determination of ergot alkaloids in animal feedingstuffs with high performance liquid chromatography - fluorescence detection

• Autorzy: Kowalczyk E. , Patyra E. , Grelik A. , Kwiatek K.
• Języki publikacji: EN

Abstrakty

EN

A high performance liquid chromatography combined with fluorescence detection (HPLC-FLD) method was developed for determination of five ergot alkaloids (EA): ergometrine, ergotamine, ergocornine, ergocrypine and ergocristine in animal feedingstuffs. The method was based on the application of QuEChERS salts for extraction and modified QuEChERS dispersive SPE for the cleanup step. Alkaloids separation was performed on a C18, 250 mm x 4.6 mm, 5 μm column with the mobile phase containing ammonium carbonate and acetonitrile. The excitation and emission wavelengths were 330 and 420 nm respectively. The method was validated according to the Commission Decision 2002/657/EC and all parameters are in agreement with the requirements of the Decision. Linearity was determined for the concentration range of 25-400 μg/kg. The coefficient of determination (R2) for all curves was from 0.985 to 0.996. The limit of detection (LOD) was in the range 3.23 to 6.53 μg/kg and the limit of quantification (LOQ) from 11.78 to 13.06 μg/kg. The decision limit (CCα) ranged from 29.56 to 43.08 μg/kg and detection capability (CCβ) from 40.65 to 51.01 μg/kg. The highest coefficient of variation (CV) for repeatability was 14.3% and for reproducibility 15.4%.

• Wydawca: -
• Czasopismo: Polish Journal of Veterinary Sciences
• Rocznik: 2016
• Tom: 19
• Numer: 3
• Opis fizyczny: p.559-565,fig.,ref.

Twórcy

autor

Kowalczyk E.

• Department of Hygiene of Animal Feedingstuffs, National Veterinary Research Institute, Partyzantow 57, 24-100 Pulawy, Poland

autor

Patyra E.

• Department of Hygiene of Animal Feedingstuffs, National Veterinary Research Institute, Partyzantow 57, 24-100 Pulawy, Poland

autor

Grelik A.

• Department of Hygiene of Animal Feedingstuffs, National Veterinary Research Institute, Partyzantow 57, 24-100 Pulawy, Poland

autor

Kwiatek K.

• Department of Hygiene of Animal Feedingstuffs, National Veterinary Research Institute, Partyzantow 57, 24-100 Pulawy, Poland

Bibliografia

• Bryła M, Szymczyk K, Jędrzejczak R, Roszko M (2015) Application of Liquid Chromatography/Ion Trap Mass Spectromery Technique to Determine Ergot Alkaloids in Grain Products. Food Technol Biotechnol 53: 16-26.
• Craig AM, Klotz JL, Duringer JM (2015) Cases of ergotism in livestock and associated ergot alkaloid concentrations in feed. Front Chem 3: 1-6.
• Crews C (2015) Analysis of Ergot Alkaloids. Toxins 7: 2024-2050.
• Di Mavungu JD, Malysheva SV, Sanders M, Larionova D, Robbens J, Dubruel P, Van Peteghem C, De Saeger S (2012) Development and validation of a new LC-MS/MS method for the simultaneous determination of six major ergot alkaloids and their corresponding epimers. Application to some food and feed commodities. Food Chem 135: 292-303.
• Directive 2002/32/EC of the European Parliament and of the Council of 7 May 2002 on undesirable substances in animal feed. http://eur-lex.europa.eu/LexUriServ/LexUri Serv.do?uri=CONSLEG:2002L0032:20100302:EN:PDF
• European Commission. 2012/154/EU: Commission recommendation of 15 March 2012 on the monitoring of the presence of ergot alkaloids in feed and food. http://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32012H0154&from=PL
• European Food Safety Authority (EFSA) (2005) Opinion of the Scientific Panel on Contaminants in Food Chain on a request from the Commission related to ergot as undesirable substance in animal feed. EFSA J 225: 1-27.
• European Food Safety Authority (EFSA), Panel on Contaminants in the Food Chain (CONTAM) (2012) Scientific Opinion on Ergot alkaloids in food and feed. EFSA J 2798: 1-158.
• Flieger M, Wurst M, Shelby R (1997) Ergot Alkaloids – Sources, Structures and Analytical Methods. Folia Microbiol 42: 3-29.
• Haarmann T, Rolke Y, Giesbert S, Tudzynski P (2009) Ergot: from witchcraft to biotechnology. Mol Plant Pathol 10: 563-577.
• Krska R, Crews C (2008) Significance, chemistry and determination of ergot alkaloids: a review. Food Addit Contam A 25: 722-731.
• Krska R, Stubbings G, Macarthur R, Crews C (2008) Simultaneous determination of six major ergot alkaloids and their epimers in cereals and foodstuffs by LC-MS-MS. Anal Bioanal Chem 391: 563-576.
• Mohamed R, Gremaud E, Richoz-Payot J, Tabet JC, Guy PA (2006) Quantitative determination of five ergot alkaloids in rye flour by liquid chromatography-electrospray ionisation tandem mass spectrometry. J Chromatogr A 1114: 62-72.
• Muller C, Kemmlein S, Klaffke H, Krauthause W, Preiss-Weigert A, Wittkowski R (2009) A basic tool for risk assessment: a new method for the analysis of ergot alkaloids in rye and selected rye products. Mol Nutr Food Res 53: 500-507.
• Ruhland M, Tischler J (2008) Determination of ergot alkaloids in feed by HPLC. Mycotoxin Res 24: 73-79.
• Storm ID, Rasmussen PH, Strobel BW, Hansen HC (2008) Ergot alkaloids in rye flour determined by solid-phase cation-exchange and high-pressure liquid chromatography with fluorescence detection. Food Addit Contam A 25: 338-346.
• Walker K, Duringer J, Craig AM (2015) Determination of the Ergot Alkaloid Ergovaline in Tall Fescue Seed and Straw Using a QuEChERS Extraction Method with High-Performance Liquid Chromatography-Fluorescence Detection. J Agric Food Chem 63: 4236-4242.

Identyfikatory

DOI

10.1515/pjvs-2016-0070