6533b7cffe1ef96bd12598c1

RESEARCH PRODUCT

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

Laura EscriváLara ManyesGuillermina FontHouda Berrada

subject

AdultHealth Toxicology and MutagenesisLiquid-Liquid Extractionlcsh:MedicineUrineToxicology01 natural sciencesArticlechemistry.chemical_compound0404 agricultural biotechnologyTandem Mass SpectrometrymycotoxinsLc ms msHealthy volunteersHumansLC-MS/MSMycotoxinReproducibilityChromatographymycotoxins; urine; optimization; method validation; LC-MS/MSlcsh:R010401 analytical chemistryExtraction (chemistry)method validation04 agricultural and veterinary sciencesRepeatability040401 food scienceurine0104 chemical scienceschemistryExtraction methodsoptimizationChromatography Liquid

description

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.

yearjournalcountryeditionlanguage
2017-10-01Toxins
https://doi.org/10.3390/toxins9100330