Automated high-throughput method using solid-phase microextraction–liquid chromatography–tandem mass spectrometry for the determination of ochratoxin A in human urine
Autor: | Carlo G. Zambonin, Dajana Vuckovic, R. Vatinno, J. J. Pawliszyn |
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Rok vydání: | 2008 |
Předmět: |
Detection limit
Chromatography Chemistry Organic Chemistry Reproducibility of Results General Medicine Tandem mass spectrometry Solid-phase microextraction Ochratoxins Sensitivity and Specificity Biochemistry High-performance liquid chromatography Analytical Chemistry Matrix (chemical analysis) Automation chemistry.chemical_compound Tandem Mass Spectrometry Liquid chromatography–mass spectrometry Humans Sample preparation Ochratoxin Solid Phase Microextraction Chromatography Liquid |
Zdroj: | Journal of Chromatography A. 1201:215-221 |
ISSN: | 0021-9673 |
DOI: | 10.1016/j.chroma.2008.05.079 |
Popis: | A new automated, high-throughput method for the determination of ochratoxin A (OTA) in human urine samples has been optimized and validated using solid-phase microextraction coupled to liquid chromatography-tandem mass spectrometry (SPME–LC–MS/MS). High-throughput was achieved by simultaneous preparation of up to 96 samples using multi-fiber SPME device and multi-well plates. A carbon-tape coating was chosen for the first time as the best extracting phase for this contaminant. The proposed method required only minimal sample pre-treatment to adjust sample pH to 3.0 using a dilution (1:1) with 0.5 M phosphate-buffered saline. A simple gradient guaranteed a good chromatographic separation from matrix interferences in only 8 min. Relative recovery (%), precision and linearity validation results met Food and Drug Administration acceptance criteria at three concentration levels (1, 10, and 50 ng/mL), indicating excellent performance of the proposed method. Limits of detection and quantitation were 0.3 and 0.7 ng/mL in urine, respectively. OTA determination in urine is a good marker for human exposure to this mycotoxin. It is also less invasive than blood analysis. This method is fully automated and the SPME technique is simpler, less time-consuming and cheaper compared with most widely adopted clean-up procedures for OTA extraction from urine. |
Databáze: | OpenAIRE |
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