Patulin in apple and apple juice: Method development, validation by liquid chromatography-tandem mass spectrometry and survey in Brazilian south supermarkets

• Published in: Journal of food composition and analysis Vol. 82; p. 103242
• Main Authors: Dias, Jonatan V., da Silva, Rosselei C., Pizzutti, Ionara R., dos Santos, Ingrid D., Dassi, Micheli, Cardoso, Carmem D.
• Format: Journal Article
• Language: English
• Published: Elsevier Inc 01.09.2019
• Subjects: Fruits; Mycotoxins; Negative ionization; Processed products; UPLC-MS/MS; Patulin: (PubChem CID: 4696); UPLC-MS/MS; Processed products; Negative ionization; Mycotoxins; Fruits
• ISSN: 0889-1575; 1096-0481
• DOI: 10.1016/j.jfca.2019.103242

•A novel method for patulin determination in apple and apple juice is presented.•The method showed to be accurate and precise for both matrices.•A survey of patulin was carried out in samples collected in Southern Brazilian supermarkets.•Apple samples showed less contamination than apple juices samples. In this work, a novel single method for patulin determination in apple and apple juice employing liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) is presented. Samples were extracted employing ethyl acetate acidified with acetic acid followed by sodium sulfate addition. The extracts were submitted to dispersive solid phase clean-up employing sodium sulfate and silica gel. The method was validated assessing linearity and linearity range, limits of detection and quantification, matrix effect, precision (RSD%) and accuracy (recovery from samples spiked at 25, 50 and 100 μg kg−1). The method showed to be suitable for patulin determination as the recovery ranged from 76 to 84% for apple and from 102 to 108% for apple juice, in both cases with RSD lower than 15%. Matrix effect was also evaluated and showed to be less intense for apple juice (−22%) than for apples (−42%). The validated method was applied to 62 samples (apple and apple juice) collected in supermarkets of southern Brazil, during the years 2016 and 2017. Apple samples showed contamination ranging from < LOQ to 757 μg kg−1 and apple juice from < LOQ to 1298 μg L−1.