INTRODUCTION AND OBJECTIVES

The presence of mycotoxins residues in pollen pose a potential risk to human health (1). In this study we performed a multiresidue method for the determination of ten mycotoxins, including patulin, zearalenone and eight trichothecenes (nivalenol, fusarenon-x, diacetoxyscirpenol,3-acetyl-deoxynivalenol,neosolaniol,deoxynivalenol, T-2 and HT-2) in pollen using gas chromatography coupled to mass spectrometry. The aim of the study was to optimize and validate the test procedure according to the criteria set by Commission Decision EU (2).

Mean results shown recoveries between 70% and 120% with RSD ≤ 20%. The method gives quantitative results for the assayed mycotoxins, providing good validation parameters in terms of linearity, trueness, precision and LOQ (table 1). Although strong matrix effect was observed, it was successfully compensated using matrix-matched calibration.

Mycotoxins were extracted from pollen samples using a QuEChERS-based extraction procedure (acronym of Quick, Easy, Cheap, Effective, Rugged and Safe) without applying any further clean-up step. The conditions of extraction, chromatography and detection have been optimized to increase the sensitivity of the method . The technique is based on the modification of the QuEChERS sample preparation (figure 1). Chromatographic determination was carried out using a GC system Agilent 7890A coupled with an Agilent 7000A triple quadrupole (QqQ) mass spectrometer.

Development of a fast multiresidue method for the determination of mycotoxinsin pollen samples using QuEChERS based method and gas chromatography

coupled to mass spectrometry

Ionela Daniela Morariu 1, Elena Corina Şchiriac2, Rodica Cuciureanu1

1University of Medicine and Pharmacy “Grigore T.Popa”, Faculty of Pharmacy, Iasi, Romania2Investigatii Medicale Praxis, Iasi, Romania

MATERIAL AND METHODS

RESULTS

CONCLUSIONS

REFERENCE

The developed method based on QuEchERS extraction procedure followed by a confirmation and quantification by gas chromatography coupled to mass spectrometry was validated and optimized for the determination of ten mycotoxins in twelve samples pollen. The optimizated method is presented as a useful tool to evaluate risk assessemnet of this multiclass mycotoxin in this pollen matrix (3).Therefore the knowledge of the occurrence of all mycotoxins should be considered a challenge in exposure assessement studies.

1. Bonvehi, J. S., & Jordà, R. E. (1997). Nutrient composition and microbiological quality of honeybee-collected pollen in Spain. Journal Agricultural Food Chemistry, 45, 725 - 732.

2. Commission Regulation, 2002b. No. 472/2002 of 12 March 2002 amending Regulation (EC) No. 466/2001 setting maximum levels for certain contaminants in foodstuffs. Official Journal of the European Communities, L 75, 16/03/2002 (pp. 18–20).

3. PDRHealth. 2005 Bee pollen. Available at: http://www.pdrhealth.com/drug_info/nmdrugprofiles/nutsupdrugs/bee_0030.shtml.