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Development of a Rapid LC-MS/MS Method for the Determination of Emerging Fusarium mycotoxins Enniatins and Beauvericin in Human Biological Fluids.

Belén Serrano A, Capriotti AL, Cavaliere C, Piovesana S, Samperi R, Ventura S, Laganà A - Toxins (Basel) (2015)

Bottom Line: The optimized SPE method was performed on graphitized carbon black cartridges after suitable dilution of the extracts, which allowed high mycotoxin absolute recoveries (76%-103%) and the removal of the major interferences from the matrix.The method was extensively evaluated for plasma and urine samples separately, providing satisfactory results in terms of linearity (R² of 0.991-0.999), process efficiency (>81%), trueness (recoveries between 85% and 120%), intra-day precision (relative standard deviation, RSD < 18%), inter-day precision (RSD < 21%) and method quantification limits (ranging between 20 ng·L(-1) and 40 ng·L(-1) in plasma and between 5 ng·L(-1) and 20 ng·L(-1) in urine).Finally, the highly sensitive validated method was applied to some urine and plasma samples from different donors.

View Article: PubMed Central - PubMed

Affiliation: Laboratorio de Toxicología, Departament de Medicina Preventiva I Salut Pública, Ciències de l'Alimentació, Toxicologia I Medicina Legal Facultat de Farmàcia, Universitat de València, València 46010, Spain. A.Belen.Serrano@uv.es.

ABSTRACT
A novel method for the simultaneous determination of enniatins A, A1, B and B1 and beauvericin, both in human urine and plasma samples, was developed and validated. The method consisted of a simple and easy pretreatment, specific for each matrix, followed by solid phase extraction (SPE) and detection by high performance liquid chromatography-tandem mass spectrometry with an electrospray ion source. The optimized SPE method was performed on graphitized carbon black cartridges after suitable dilution of the extracts, which allowed high mycotoxin absolute recoveries (76%-103%) and the removal of the major interferences from the matrix. The method was extensively evaluated for plasma and urine samples separately, providing satisfactory results in terms of linearity (R² of 0.991-0.999), process efficiency (>81%), trueness (recoveries between 85% and 120%), intra-day precision (relative standard deviation, RSD < 18%), inter-day precision (RSD < 21%) and method quantification limits (ranging between 20 ng·L(-1) and 40 ng·L(-1) in plasma and between 5 ng·L(-1) and 20 ng·L(-1) in urine). Finally, the highly sensitive validated method was applied to some urine and plasma samples from different donors.

No MeSH data available.


Structures of the investigated mycotoxins, namely enniatin A (ENA), enniatin A1 (ENA1), enniatin B (ENB), enniatin B1 (ENB1) and beauvericin (BEA); R1, R2, and R3 can be sec-butyl (s-Bu), isopropyl (i-Pr) or benzyl (Bn) groups.
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toxins-07-03554-f001: Structures of the investigated mycotoxins, namely enniatin A (ENA), enniatin A1 (ENA1), enniatin B (ENB), enniatin B1 (ENB1) and beauvericin (BEA); R1, R2, and R3 can be sec-butyl (s-Bu), isopropyl (i-Pr) or benzyl (Bn) groups.

Mentions: Taking into account the lack of methodology for the extraction of ENs and BEA from human biological fluids, the main aim of this work was the development of a reliable and sensitive analytical method for the simultaneous determination of the main four ENs and BEA (see Figure 1) by LC-MS/MS applicable to human urine and plasma. To achieve this goal, an extraction method specific for the biological fluid, followed by a cleanup based on SPE, was optimized for urine and plasma samples. Finally, after validation, the applicability of the optimized method was demonstrated by the analysis of human samples of urine and plasma.


Development of a Rapid LC-MS/MS Method for the Determination of Emerging Fusarium mycotoxins Enniatins and Beauvericin in Human Biological Fluids.

Belén Serrano A, Capriotti AL, Cavaliere C, Piovesana S, Samperi R, Ventura S, Laganà A - Toxins (Basel) (2015)

Structures of the investigated mycotoxins, namely enniatin A (ENA), enniatin A1 (ENA1), enniatin B (ENB), enniatin B1 (ENB1) and beauvericin (BEA); R1, R2, and R3 can be sec-butyl (s-Bu), isopropyl (i-Pr) or benzyl (Bn) groups.
© Copyright Policy
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4591648&req=5

toxins-07-03554-f001: Structures of the investigated mycotoxins, namely enniatin A (ENA), enniatin A1 (ENA1), enniatin B (ENB), enniatin B1 (ENB1) and beauvericin (BEA); R1, R2, and R3 can be sec-butyl (s-Bu), isopropyl (i-Pr) or benzyl (Bn) groups.
Mentions: Taking into account the lack of methodology for the extraction of ENs and BEA from human biological fluids, the main aim of this work was the development of a reliable and sensitive analytical method for the simultaneous determination of the main four ENs and BEA (see Figure 1) by LC-MS/MS applicable to human urine and plasma. To achieve this goal, an extraction method specific for the biological fluid, followed by a cleanup based on SPE, was optimized for urine and plasma samples. Finally, after validation, the applicability of the optimized method was demonstrated by the analysis of human samples of urine and plasma.

Bottom Line: The optimized SPE method was performed on graphitized carbon black cartridges after suitable dilution of the extracts, which allowed high mycotoxin absolute recoveries (76%-103%) and the removal of the major interferences from the matrix.The method was extensively evaluated for plasma and urine samples separately, providing satisfactory results in terms of linearity (R² of 0.991-0.999), process efficiency (>81%), trueness (recoveries between 85% and 120%), intra-day precision (relative standard deviation, RSD < 18%), inter-day precision (RSD < 21%) and method quantification limits (ranging between 20 ng·L(-1) and 40 ng·L(-1) in plasma and between 5 ng·L(-1) and 20 ng·L(-1) in urine).Finally, the highly sensitive validated method was applied to some urine and plasma samples from different donors.

View Article: PubMed Central - PubMed

Affiliation: Laboratorio de Toxicología, Departament de Medicina Preventiva I Salut Pública, Ciències de l'Alimentació, Toxicologia I Medicina Legal Facultat de Farmàcia, Universitat de València, València 46010, Spain. A.Belen.Serrano@uv.es.

ABSTRACT
A novel method for the simultaneous determination of enniatins A, A1, B and B1 and beauvericin, both in human urine and plasma samples, was developed and validated. The method consisted of a simple and easy pretreatment, specific for each matrix, followed by solid phase extraction (SPE) and detection by high performance liquid chromatography-tandem mass spectrometry with an electrospray ion source. The optimized SPE method was performed on graphitized carbon black cartridges after suitable dilution of the extracts, which allowed high mycotoxin absolute recoveries (76%-103%) and the removal of the major interferences from the matrix. The method was extensively evaluated for plasma and urine samples separately, providing satisfactory results in terms of linearity (R² of 0.991-0.999), process efficiency (>81%), trueness (recoveries between 85% and 120%), intra-day precision (relative standard deviation, RSD < 18%), inter-day precision (RSD < 21%) and method quantification limits (ranging between 20 ng·L(-1) and 40 ng·L(-1) in plasma and between 5 ng·L(-1) and 20 ng·L(-1) in urine). Finally, the highly sensitive validated method was applied to some urine and plasma samples from different donors.

No MeSH data available.