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Toxins 2017, 9(10), 330; https://doi.org/10.3390/toxins9100330

Mycotoxin Analysis of Human Urine by LC-MS/MS: A Comparative Extraction Study

Laboratory of Food Chemistry and Toxicology, Faculty of Pharmacy, University of Valencia, Av. Vicent Andres Estelles s/n, 46100 Burjassot, Spain
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Academic Editor: Aldo Laganà
Received: 29 September 2017 / Revised: 13 October 2017 / Accepted: 15 October 2017 / Published: 19 October 2017
(This article belongs to the Section Mycotoxins)
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Abstract

The lower mycotoxin levels detected in urine make the development of sensitive and accurate analytical methods essential. Three extraction methods, namely salting-out liquid–liquid extraction (SALLE), miniQuEChERS (quick, easy, cheap, effective, rugged, and safe), and dispersive liquid–liquid microextraction (DLLME), were evaluated and compared based on analytical parameters for the quantitative LC-MS/MS measurement of 11 mycotoxins (AFB1, AFB2, AFG1, AFG2, OTA, ZEA, BEA, EN A, EN B, EN A1 and EN B1) in human urine. DLLME was selected as the most appropriate methodology, as it produced better validation results for recovery (79–113%), reproducibility (RSDs < 12%), and repeatability (RSDs < 15%) than miniQuEChERS (71–109%, RSDs <14% and <24%, respectively) and SALLE (70–108%, RSDs < 14% and < 24%, respectively). Moreover, the lowest detection (LODS) and quantitation limits (LOQS) were achieved with DLLME (LODs: 0.005–2 μg L−1, LOQs: 0.1–4 μg L−1). DLLME methodology was used for the analysis of 10 real urine samples from healthy volunteers showing the presence of ENs B, B1 and A1 at low concentrations. View Full-Text
Keywords: mycotoxins; urine; optimization; method validation; LC-MS/MS mycotoxins; urine; optimization; method validation; LC-MS/MS
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Escrivá, L.; Manyes, L.; Font, G.; Berrada, H. Mycotoxin Analysis of Human Urine by LC-MS/MS: A Comparative Extraction Study. Toxins 2017, 9, 330.

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