Sensitive determination of cyclopiazonic acid in dry-cured ham using a QuEChERS method and UHPLC-MS/MS

Belén Peromingo; Mar Rodríguez; Félix Núñez; Antonio Silva; Alicia Rodríguez

doi:10.1016/j.foodchem.2018.04.126

Sensitive determination of cyclopiazonic acid in dry-cured ham using a QuEChERS method and UHPLC-MS/MS

Food Chem. 2018 Oct 15:263:275-282. doi: 10.1016/j.foodchem.2018.04.126. Epub 2018 Apr 30.

Authors

Belén Peromingo¹, Mar Rodríguez¹, Félix Núñez¹, Antonio Silva², Alicia Rodríguez³

Affiliations

¹ Food Hygiene and Safety, Meat and Meat Products Research Institute, Faculty of Veterinary Science, University of Extremadura, Avda. de las Ciencias, s/n, 10003 Cáceres, Spain.
² Facility of Innovation and Analysis in Animal Source Foodstuffs of SAIUEx, University of Extremadura, Avda. de las Ciencias, s/n, 10003 Cáceres, Spain.
³ Food Hygiene and Safety, Meat and Meat Products Research Institute, Faculty of Veterinary Science, University of Extremadura, Avda. de las Ciencias, s/n, 10003 Cáceres, Spain. Electronic address: aliciarj@unex.es.

PMID: 29784317
DOI: 10.1016/j.foodchem.2018.04.126

Abstract

An extraction method and an UHPLC-MS/MS method for the quantification of CPA in dry-cured ham were developed and validated. To optimise detection and quantification of CPA, the composition of mobile phase, flow rates, gradient-related factors and solvents used for resuspension of dry extracts were evaluated. Besides, four extraction methods were tested. The best peak shape and resolution were obtained by eluting the mobile phase consisting in acetic acid-ammonium acetate buffer pH 5.75/methanol in gradient mode at a flow rate of 0.2 mL/min. The method 4 relied on the QuEChERS methodology was the most effective one. Almost half of the 61 dry-cured ham samples examined were contaminated with CPA, with values ranging from 36.1 to 540.1 ng/g. The combination of a QuEChERS-based extraction method and analysis by UHPLC-MS/MS allows highly sensitive, fast, reliable and cheap detection and quantification of CPA for routine analysis in ham.

Keywords: Cyclopiazonic acid; Dry-cured ham; QuEChERS; UHPLC–MS/MS.

MeSH terms

Animals
Chromatography, High Pressure Liquid*
Indoles / analysis*
Indoles / isolation & purification
Limit of Detection
Meat Products / analysis*
Reproducibility of Results
Solid Phase Extraction / methods*
Swine
Tandem Mass Spectrometry*

Substances

Indoles
cyclopiazonic acid