Determination of malachite green residues in fish using molecularly imprinted solid-phase extraction followed by liquid chromatography-linear ion trap mass spectrometry |
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Authors: | María Jesús Martínez Bueno Ana Uclés María Dolores Hernando Olga Shimelis Amadeo R Fernández-Alba |
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Institution: | a Pesticide Residues Research Group, Department of Hydrogeology and Analytical Chemistry, University of Almería, 04120 La Cañada de San Urbano, Almería, Spain b National Reference Centre for Persistent Organic Pollutants, University of Alcalá, 28871 Alcalá de Henares, Madrid, Spain c SUPELCO, 595 North Harrison Road, Bellefonte, PA 16823, USA d MIP Technologies AB, Box 737, Scheelevägen 22, 220 07 Lund, Sweden e Fundación IMDEA-Agua, C/ Punto Net 4, 2ª planta, Edificio ZYE, Parque Científico Tecnológico de la Universidad de Alcalá 28805, Alcalá de Henares, Madrid, Spain |
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Abstract: | This paper describes the development of an analytical procedure to determine malachite green (MG) residues in salmon samples using molecularly imprinted polymers (MIPs) as the extraction and clean-up material, followed by liquid chromatography-linear ion trap mass spectrometry (LC-QqQLIT-MS/MS). MG and two structurally related compounds, crystal violet (CV) and brilliant green (BG) were employed for the selectivity test. The imprinted polymers exhibited high binding affinity for MG, while CV and BG showed less binding capacity: 47% and 34%, respectively. The recovery values of MG in salmon samples fortified with leucomalachite green (LMG) were determined by measuring the amount of MG in the sample, after carrying out the oxidation reaction with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), which converts the LMG back into chromic-form. The average recovery of MG in spiked salmon muscle over the concentration range 1-100 ng g−1 was 98% with a relative standard deviation value (R.S.D.) below 12%. The method detection limits (MDLs) obtained for MG, CV, BG and their leuco-metabolites were in the range of 3-20 ng kg−1 (ppt). |
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Keywords: | Molecularly imprinted polymers (MIPs) Malachite green Crystal violet Brilliant green Leuco-metabolites Fish Liquid chromatography mass spectrometry (LC-MS) |
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