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| Fast Determination of Residues of Carbofuran and Its Metabolite in Animal Tissues by Liquid Chromatography with Tandem Mass Spectrometry |
| YANG Ting, LÜ Yan, CHEN Guo, WU Yinliang* |
| The Ningbo Academy of Agricultural Sciences, Ningbo 315040, China |
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Abstract A method for determining residues of carbofuran and its metabolite 3-hydroxycarbofuran in animal tissues was
developed by liquid chromatography with tandem mass spectrometry. Samples were extracted with acetonitrile. Then the
extract was purified by dispersive solid phase extraction method using PSA and C18 as sorbents. After purification, the extract
was dried under nitrogen stream and the residue was dissolved in 0.1% formic acid solution/acetonitrile mixture (50/50, V/V)
and filtered through a 0.22 μm filter and 10 μL of the filtrate was injected into the LC system for analysis. The analysis
was performed on an Acquity BEH C18 column with a mixture of 0.1% formic acid solution and acetonitrile as the mobile
phase under gradient elution conditions. The mass spectrometer was operated in multiple reaction monitoring (MRM) mode
with positive ion electrospray ionization (ESI). The analytes were quantified with the isotope internal standard dilution
method. Good linearity was obtained for carbofuran and 3-hydroxycarbofuran in the concentration range of 0.05–25.0 and
0.25–50.0 μg/L with correlation coefficients more than 0.999, respectively. The recoveries in animal tissues (pork and beef)
were 95.7%–107.0% at fortified levels of 0.25–10 μg/kg with limits of detection of 0.10 and 0.50 μg/kg and limits of quantitation
of 0.25 and 1.0 μg/kg for carbofuran and 3-hydroxycarbofuran, respectively. The relative standard deviations of intra- and interbatch
assays were between 3.2% and 5.9%, and between 4.5% and 6.6%, respectively. The method was demonstrated to be suitable
for the fast determination of residues of carbofuran and its metabolite 3-hydroxycarbofuran in animal tissues.
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