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Title: Overcoming matrix effects in electrospray: Quantitation of β-agonists in complex matrices by isotope dilution liquid chromatography-mass spectrometry using singly <sup>13</sup>C-labeled analogues
Authors: González-Antuña, Ana 
Domínguez-Romero, Juan C.
García-Reyes, Juan F.
Rodríguez-González, Pablo
Centineo, Giuseppe
García Alonso, J. Ignacio
Molina-Díaz, Antonio
UNESCO Clasification: 32 Ciencias médicas
230103 Análisis cromatográfico
230110 Espectroscopia de masas
Keywords: Electrospray
Chromatography-mass spectrometry
Issue Date: 2013
Journal: Journal of Chromatography A 
Abstract: In this work, the implementation of isotope dilution mass spectrometry (IDMS) using minimal labeling and isotope pattern deconvolution (IPD) is evaluated as a strategy for the minimization of matrix effects during trace determination of β2-agonists in complex matrices by liquid chromatography electrospray ionization mass spectrometry (LC-ESI-MS). First, the parameters affecting the measurement of isotopic composition of organic compounds by liquid chromatography electrospray ionization high resolution mass spectrometry with a time-of-flight analyzer were evaluated using as a case of study three different β2-agonists: clenbuterol, clenproperol and brombuterol. Then, a calibration graph-free IDMS methodology was evaluated in order to overcome matrix effects in LC-ESI-MS in complex samples. In this procedure singly (13)C-labeled analogues of clenbuterol, clenproperol and brombuterol were employed in combination with IPD. Using this approach accurate and precise results were obtained in the simultaneous quantification of β2-agonists in human urine and bovine liver, even at the sub ngg(-1) and particularly in spite of the previously reported matrix effects. Recovery rates in the range of 97-114% in fortified human urine and from 95% to 111% in fortified bovine liver were obtained with RSD (%) of independent recovery experiments always lower than 6%. These results demonstrate that the proposed methodology based on the use of (13)C1-labeled standards and IPD is a reliable approach for accurate LC-MS quantitation of small molecules and compatible with full-scan high-resolution mass spectrometry.
ISSN: 0021-9673
DOI: 10.1016/j.chroma.2013.02.074
Source: Journal of Chromatography A [ISSN 0021-9673],v. 1288, p. 40-47 (Mayo 2013)
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