4.6 Article

Determination of benzimidazoles in meat samples by capillary zone electrophoresis tandem mass spectrometry following dispersive liquid-liquid microextraction

Journal

JOURNAL OF CHROMATOGRAPHY A
Volume 1490, Issue -, Pages 212-219

Publisher

ELSEVIER
DOI: 10.1016/j.chroma.2017.02.023

Keywords

Benzimidazoles; Capillary electrophoresis; Dispersive liquid-liquid micro extraction; Mass spectrometry; Meat samples

Funding

  1. ndalusian Government (Junta de Andalucia) [P12-AGR-1647]
  2. MINECO [JCI-2014-19573]
  3. Andalucia Talent Hub Program
  4. European Union's Seventh Framework Program, Marie Skkodowska-Curie actions (COFUND) [291780]
  5. Ministry of Economy, Innovation, Science and Employment of the Junta de Andalucia

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A novel method based on capillary zone electrophoresis-tandem mass spectrometry has been proposed and validated for the identification and simultaneous quantification of twelve benzimidazoles in meat samples. Electrophoretic separation was carried out using 500 mM formic acid (pH 2.2) as background electrolyte and applying a voltage of 25 kV at 25 degrees C. In order to improve the sensitivity, stacking mode injection was applied, using as injection solvent a mixture of 30:70 acetonitrile/water at 50 mbar for 75 s. Sensitivity enhancement factors from 74 to 317 were obtained under these conditions. Detection using an ion trap as analyzer, operating in multiple reactions monitoring mode was employed. The main MS/MS parameters as well as the composition of the sheath liquid and other electrospray variables were optimized in order to obtain the highest sensitivity and precision in conjunction with an unequivocal identification. The method was applied to poultry and pork muscle samples. The deproteinization of samples and extraction of benzimidazoles was carried out with acetonitrile. MgSO4 and NaCI were added as salting-out agents. Subsequently, dispersive liquid-liquid microextraction was applied as clean up procedure. The organic layer (acetonitrile, used as dispersant) containing the benzimidazoles was mixed with the extractant (chloroform) and both were injected in water, producing a cloudy solution. Recoveries for fortified samples were higher than 70%, with relative standard deviations lower than 16% were obtained in all cases. The limits of detection were below 3 mu g kg(-1), demonstrating the applicability of this fast, simple, and environmentally friendly method. (C) 2017 Elsevier B.V. All rights reserved.

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