Development and validation of a QuEChERS method coupled to liquid chromatography and high resolution mass spectrometry to determine pyrrolizidine and tropane alkaloids in honey

Marianna Martinello; Alice Borin; Roberto Stella; Davide Bovo; Giancarlo Biancotto; Albino Gallina; Franco Mutinelli

doi:10.1016/j.foodchem.2017.04.186

Development and validation of a QuEChERS method coupled to liquid chromatography and high resolution mass spectrometry to determine pyrrolizidine and tropane alkaloids in honey

Food Chem. 2017 Nov 1:234:295-302. doi: 10.1016/j.foodchem.2017.04.186. Epub 2017 May 2.

Authors

Marianna Martinello¹, Alice Borin², Roberto Stella³, Davide Bovo³, Giancarlo Biancotto³, Albino Gallina⁴, Franco Mutinelli²

Affiliations

¹ National Reference Laboratory for Beekeeping, Istituto Zooprofilattico Sperimentale delle Venezie, Padova, Italy. Electronic address: mmartinello@izsvenezie.it.
² National Reference Laboratory for Beekeeping, Istituto Zooprofilattico Sperimentale delle Venezie, Padova, Italy.
³ Department of Chemistry, Istituto Zooprofilattico Sperimentale delle Venezie, Padova, Italy.
⁴ National Reference Laboratory for Beekeeping, Istituto Zooprofilattico Sperimentale delle Venezie, Padova, Italy; Department of Chemistry, Istituto Zooprofilattico Sperimentale delle Venezie, Padova, Italy.

PMID: 28551239
DOI: 10.1016/j.foodchem.2017.04.186

Abstract

Awareness about pyrrolizidine alkaloids (PAs) and tropane alkaloids (TAs) in food was recently raised by the European Food Safety Authority stressing the lack of data and gaps of knowledge required to improve the risk assessment strategy. The present study aimed at the elaboration and validation of a method to determine PAs and TAs in honey. QuEChERS sample treatment and liquid chromatography coupled to hybrid high resolution mass spectrometry, were used. The method resulted in good linearity (R²>0.99) and low limits of detection and quantification, ranging from 0.04 to 0.2µgkg^-1 and from 0.1 to 0.7µgkg^-1 respectively. Recoveries ranged from 92.3 to 114.8% with repeatability lying between 0.9 and 15.1% and reproducibility between 1.1 and 15.6%. These performances demonstrate the selectivity and sensitivity of the method for simultaneous trace detection and quantification of PAs and TAs in honey, verified through the analysis of forty commercial samples.

Keywords: Atropine (PubChem CID: 174174); Echimidine (PubChem CID: 5281729); Food contaminants; HRMS; Heliotrine (PubChem CID: 906426); Honey; Intermedine (PubChem CID: 114843); Lasiocarpine (PubChem CID: 5281735); Lycopsamine (PubChem CID: 107938); Pyrrolizidine alkaloids; Retrorsine (PubChem CID: 5281743); Scopolamine (PubChem CID: 3000322); Senecionine (PubChem CID: 5280906); Seneciphylline (PubChem CID: 5281750); Tropane alkaloids; Validation.

Publication types

Validation Study

MeSH terms

Chromatography, Liquid
Food Contamination / analysis*
Honey / analysis*
Pyrrolizidine Alkaloids / analysis*
Reproducibility of Results
Tandem Mass Spectrometry
Tropanes / analysis*

Substances

Pyrrolizidine Alkaloids
Tropanes