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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 β-agonists 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. | URI: | http://hdl.handle.net/10553/45332 | 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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