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

Peromingo, Belén, Rodríguez, Mar, Núñez, Félix, Silva, Antonio, Rodríguez, Alicia
Food chemistry 2018 v.263 pp. 275-282
acetic acid, ammonium acetate, buffer index, buffers, cured meats, cyclopiazonic acid, ham, pH, solvents, tandem mass spectrometry
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.