Romanian Society of Pharmaceutical Sciences
 

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DETERMINATION OF OCHRATOXIN A IN FOOD BY LC-MS/MS

ANCA VARTOLOMEI1, LAURIAN VLASE2, MAGDALENA CUCIUREANU3*, RODICA CUCIUREANU1, DANIEL SAVETA POPA4

1.Department of Environmental and Food Chemistry, Faculty of Pharmacy, University of Medicine and Pharmacy “Grigore T. Popa” Iaşi, 16 Universităţii, 700115– Iaşi, Romania
2 .Department of Pharmaceutical Technology and Biopharmacy, Faculty of Pharmacy, University of Medicine and Pharmacy “Iuliu Haţieganu” Cluj-Napoca, 8 Victor Babeş, 400012 – Cluj-Napoca, Romania
3 .Department of Pharmacology, Faculty of Dental Medicine, University of Medicine and Pharmacy “Grigore T. Popa” Iaşi, 16 Universităţii, 700115– Iaşi, Romania
4 .Department of Toxicology, Faculty of Pharmacy, University of Medicine and Pharmacy “Iuliu Haţieganu” Cluj-Napoca, 8 Victor Babeş, 400012 – Cluj-Napoca, Romania

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A liquid chromatographic – tandem mass spectrometry (LC-MS/MS) method for quantification of ochratoxin A (OTA) in foods was developed and validated. OTA is a mycotoxin which can contaminate food in semitropical and temperate climates. It has nephrotoxic, genotoxic, carcinogenic, teratogenic and neurotoxic potential. The chromatographic separation was performed on a Zorbax SB-C18 column with gradient elution using a mobile phase of acetonitrile and 0.1% (v/v) acetic acid in water at 48 ºC with a flow rate of 1 mL/min. The detection of OTA was performed in MRM mode using an ESI source in negative mode. The monitored transition was m/z 402 → (358 + 359 + 360). Samples of bread, dry fruit, breakfast cereals, spices, beer, cereals, and seeds were analyzed. OTA was extracted from the food samples in a mixture of ethyl acetate : methanol : acetic acid (95:5:0.5, v/v/v) after solubilization in aqueous acidic medium and cleanup on celite. The elaborated method showed a good linearity (r > 0.998), precision (CV < 10.0 %) and accuracy (bias < 9.7 %) over the range of concentrations studied (0.45-36 ng/mL) and a good sensitivity (LLOQ of 0.45 ng/mL). The run-time of chromatographic analysis was 18 min and the retention time of OTA 13 min. The developed and validated method is simple and efficient, and can be applied in the monitoring of food safety and assessment of exposure to OTA through food.