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

Overview

Journal Toxins (Basel)

Publisher MDPI

Specialty Toxicology

Date 2017 Oct 20

PMID 29048356

Citations 14

Authors

Laura Escriva

Lara Manyes

Guillermina Font

Houda Berrada

Affiliations

Soon will be listed here.

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, LOQs: 0.1-4 μg L). 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.

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References

Warth B, Sulyok M, Krska R . LC-MS/MS-based multibiomarker approaches for the assessment of human exposure to mycotoxins. Anal Bioanal Chem. 2013; 405(17):5687-95. PMC: 3695324. DOI: 10.1007/s00216-013-7011-1. View

Ahn J, Kim D, Kim H, Jahng K . Quantitative determination of mycotoxins in urine by LC-MS/MS. Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2010; 27(12):1674-82. DOI: 10.1080/19440049.2010.505201. View

Rodriguez-Carrasco Y, Manes J, Berrada H, Font G . Preliminary estimation of deoxynivalenol excretion through a 24 h pilot study. Toxins (Basel). 2015; 7(3):705-18. PMC: 4379519. DOI: 10.3390/toxins7030705. View

Rubert J, Leon N, Saez C, Martins C, Godula M, Yusa V . Evaluation of mycotoxins and their metabolites in human breast milk using liquid chromatography coupled to high resolution mass spectrometry. Anal Chim Acta. 2014; 820:39-46. DOI: 10.1016/j.aca.2014.02.009. View

Mally A, Solfrizzo M, Degen G . Biomonitoring of the mycotoxin Zearalenone: current state-of-the art and application to human exposure assessment. Arch Toxicol. 2016; 90(6):1281-92. DOI: 10.1007/s00204-016-1704-0. View

Wallin S, Gambacorta L, Kotova N, Lemming E, Nalsen C, Solfrizzo M . Biomonitoring of concurrent mycotoxin exposure among adults in Sweden through urinary multi-biomarker analysis. Food Chem Toxicol. 2015; 83:133-9. DOI: 10.1016/j.fct.2015.05.023. View

Fernandez P, Regenjo M, Bermejo A, Fernandez A, Lorenzo R, Carro A . Analysis of drugs of abuse in human plasma by dispersive liquid-liquid microextraction and high-performance liquid chromatography. J Appl Toxicol. 2014; 35(4):418-25. DOI: 10.1002/jat.3035. View

Rodriguez-Carrasco Y, Molto J, Manes J, Berrada H . Exposure assessment approach through mycotoxin/creatinine ratio evaluation in urine by GC-MS/MS. Food Chem Toxicol. 2014; 72:69-75. DOI: 10.1016/j.fct.2014.07.014. View

Rodriguez-Carrasco Y, Molto J, Manes J, Berrada H . Development of microextraction techniques in combination with GC-MS/MS for the determination of mycotoxins and metabolites in human urine. J Sep Sci. 2017; 40(7):1572-1582. DOI: 10.1002/jssc.201601131. View

10.

Rodriguez-Carrasco Y, Molto J, Manes J, Berrada H . Development of a GC-MS/MS strategy to determine 15 mycotoxins and metabolites in human urine. Talanta. 2014; 128:125-31. DOI: 10.1016/j.talanta.2014.04.072. View

11.

Tolosa J, Font G, Manes J, Ferrer E . Multimycotoxin analysis in water and fish plasma by liquid chromatography-tandem mass spectrometry. Chemosphere. 2015; 145:402-8. DOI: 10.1016/j.chemosphere.2015.11.085. View

12.

Hmaissia Khlifa K, Ghali R, Mazigh C, Aouni Z, Machgoul S, Hedhili A . Ochratoxin A levels in human serum and foods from nephropathy patients in Tunisia: where are you now?. Exp Toxicol Pathol. 2010; 64(5):509-12. DOI: 10.1016/j.etp.2010.11.006. View

13.

Campone L, Piccinelli A, Celano R, Russo M, Rastrelli L . Rapid analysis of aflatoxin M1 in milk using dispersive liquid-liquid microextraction coupled with ultrahigh pressure liquid chromatography tandem mass spectrometry. Anal Bioanal Chem. 2013; 405(26):8645-52. DOI: 10.1007/s00216-013-7277-3. View

14.

Kralj Cigic I, Prosen H . An overview of conventional and emerging analytical methods for the determination of mycotoxins. Int J Mol Sci. 2009; 10(1):62-115. PMC: 2662450. DOI: 10.3390/ijms10010062. View

15.

Arroyo-Manzanares N, Gamiz-Gracia L, Garcia-Campana A . Determination of ochratoxin A in wines by capillary liquid chromatography with laser induced fluorescence detection using dispersive liquid-liquid microextraction. Food Chem. 2012; 135(2):368-72. DOI: 10.1016/j.foodchem.2012.05.009. View

16.

Huybrechts B, Martins J, Debongnie P, Uhlig S, Callebaut A . Fast and sensitive LC-MS/MS method measuring human mycotoxin exposure using biomarkers in urine. Arch Toxicol. 2014; 89(11):1993-2005. DOI: 10.1007/s00204-014-1358-8. View

17.

Song S, Njumbe Ediage E, Wu A, De Saeger S . Development and application of salting-out assisted liquid/liquid extraction for multi-mycotoxin biomarkers analysis in pig urine with high performance liquid chromatography/tandem mass spectrometry. J Chromatogr A. 2012; 1292:111-20. DOI: 10.1016/j.chroma.2012.10.071. View

18.

Escriva L, Font G, Manyes L, Berrada H . Studies on the Presence of Mycotoxins in Biological Samples: An Overview. Toxins (Basel). 2017; 9(8). PMC: 5577585. DOI: 10.3390/toxins9080251. View

19.

Campone L, Piccinelli A, Rastrelli L . Dispersive liquid-liquid microextraction combined with high-performance liquid chromatography-tandem mass spectrometry for the identification and the accurate quantification by isotope dilution assay of ochratoxin A in wine samples. Anal Bioanal Chem. 2010; 399(3):1279-86. DOI: 10.1007/s00216-010-4347-7. View