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Development and validation of an ultra-high performance liquid chromatography tandem mass spectrometry method for quantifying thyreostats in urine without derivatisation

(2010) JOURNAL OF CHROMATOGRAPHY A. 1217(26). p.4285-4293
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Abstract
Thyreostatic drugs, illegally administrated to livestock for fattening purposes, are banned in the European Union since 1981 (Council Directive 81/602/EC). For monitoring their illegal use, sensitive and specific analytical methods are required. In this study an UHPLC-MS/MS method was described for quantitative analysis of eight thyreostatic drugs in urine, this without a derivatisation step. The sample pretreatment involved a reduction step with dithiothreitol under denaturating conditions at 65 degrees C, followed by liquid-liquid extraction with ethyl acetate. This analytical procedure was subsequently validated according to the EU criteria (2002/657/EC Decision), resulting in decision limits and detection capabilities ranging between 1.1 and 5.5 mu g L-1 and 1.7 and 7.5 mu g L-1, respectively. The method obtained for all, xenobiotic thyreostats, a precision (relative standard deviation) lower than 15.5%, and the linearity ranged between 0.982 and 0.999. The performance characteristics fulfill not only the requirements of the EU regarding the provisional minimum required performance limit (100 mu g L-1), but also the recommended concentration fixed at 10 mu g L-1 in urine set by the Community of Reference Laboratories. Future experiments applying this method should provide the answer to the alleged endogenous status of thiouracil. (c) 2010 Elsevier B.V. All rights reserved.
Keywords
CONFIRMATION, THIOURACIL, SOLID-PHASE DISPERSION, GAS-CHROMATOGRAPHY, ESCHERICHIA-COLI, THYROID SAMPLES, RESIDUES, DRUGS, BOVINE, MEAT

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Chicago
Vanden Bussche, Julie, Lynn Vanhaecke, Y Deceuninck, Klaas Wille, Karen Bekaert, Bruno Le Bizec, and Hubert De Brabander. 2010. “Development and Validation of an Ultra-high Performance Liquid Chromatography Tandem Mass Spectrometry Method for Quantifying Thyreostats in Urine Without Derivatisation.” Journal of Chromatography A 1217 (26): 4285–4293.
APA
Vanden Bussche, J., Vanhaecke, L., Deceuninck, Y., Wille, K., Bekaert, K., Le Bizec, B., & De Brabander, H. (2010). Development and validation of an ultra-high performance liquid chromatography tandem mass spectrometry method for quantifying thyreostats in urine without derivatisation. JOURNAL OF CHROMATOGRAPHY A, 1217(26), 4285–4293.
Vancouver
1.
Vanden Bussche J, Vanhaecke L, Deceuninck Y, Wille K, Bekaert K, Le Bizec B, et al. Development and validation of an ultra-high performance liquid chromatography tandem mass spectrometry method for quantifying thyreostats in urine without derivatisation. JOURNAL OF CHROMATOGRAPHY A. Elsevier; 2010;1217(26):4285–93.
MLA
Vanden Bussche, Julie, Lynn Vanhaecke, Y Deceuninck, et al. “Development and Validation of an Ultra-high Performance Liquid Chromatography Tandem Mass Spectrometry Method for Quantifying Thyreostats in Urine Without Derivatisation.” JOURNAL OF CHROMATOGRAPHY A 1217.26 (2010): 4285–4293. Print.
@article{1002928,
  abstract     = {Thyreostatic drugs, illegally administrated to livestock for fattening purposes, are banned in the European Union since 1981 (Council Directive 81/602/EC). For monitoring their illegal use, sensitive and specific analytical methods are required. In this study an UHPLC-MS/MS method was described for quantitative analysis of eight thyreostatic
   drugs in urine, this without a derivatisation step. The sample pretreatment involved a reduction step with dithiothreitol under denaturating conditions at 65 degrees C, followed by liquid-liquid extraction with ethyl acetate. This analytical procedure was subsequently validated according to the EU criteria (2002/657/EC Decision), resulting in decision limits and detection capabilities ranging between 1.1 and 5.5 mu g L-1 and 1.7 and 7.5 mu g L-1, respectively. The method obtained for all, xenobiotic thyreostats, a    precision (relative standard deviation) lower than 15.5\%, and the linearity ranged between 0.982 and 0.999. The performance characteristics fulfill not only the requirements of the EU regarding the provisional minimum required performance limit (100 mu g L-1), but also the recommended concentration fixed at 10 mu g L-1 in urine set by the Community of Reference Laboratories. Future experiments applying this method should provide the answer to the alleged endogenous status of thiouracil. (c) 2010 Elsevier B.V. All rights reserved.},
  author       = {Vanden Bussche, Julie and Vanhaecke, Lynn and Deceuninck, Y and Wille, Klaas and Bekaert, Karen and Le Bizec, Bruno and De Brabander, Hubert},
  issn         = {0021-9673},
  journal      = {JOURNAL OF CHROMATOGRAPHY A},
  keyword      = {CONFIRMATION,THIOURACIL,SOLID-PHASE DISPERSION,GAS-CHROMATOGRAPHY,ESCHERICHIA-COLI,THYROID SAMPLES,RESIDUES,DRUGS,BOVINE,MEAT},
  language     = {eng},
  number       = {26},
  pages        = {4285--4293},
  publisher    = {Elsevier},
  title        = {Development and validation of an ultra-high performance liquid chromatography tandem mass spectrometry method for quantifying thyreostats in urine without derivatisation},
  url          = {http://dx.doi.org/10.1016/j.chroma.2010.04.030},
  volume       = {1217},
  year         = {2010},
}

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