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| Determination of Residual Metaldehyde in Fish Meat by Liquid Chromatography with Tandem Mass Spectrometry |
| LÜ Yan1, LIU Yongjun2, JIANG Xiaoxiao1, CHEN Guo1, WU Yinliang1,* |
| 1. Ningbo Academy of Agricultural Sciences, Ningbo 315040, China; 2. The Center for Animal Disease Control and Prevention, Beijing 100125, China |
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Abstract A method was developed for determining residual metaldehyde in fish meat by liquid chromatography with tandem mass spectrometry (LC-MS/MS). Fish meat samples were extracted with acetonitrile and sequentially purified by salting-out method followed by solid phase extraction with PSA and C18 sorbent. After dilution with 0.1% formic acid solution, the samples were analyzed by LC-MS/MS on a Waters Acquity BEH C18 column with acetonitrile/0.1 % formic acid in water as mobile phase with gradient elution. The mass spectrometer was operated using multiple reaction monitoring (MRM) in the positive ion mode. The analyte was quantified by the internal standard calibration curve method. Good linearity was obtained for metaldehyde in the concentration range of 0.05–5.0 μg/L with linear relative coefficient more than 0.999. The recoveries in fish meat were 98.5%–100.8% at fortified levels of 1.0–2.0 μg/kg with a limit of quantitation of 1.0 μg/kg for metaldehyde. The relative standard deviations of intra-assay and inter-assay were below 10%. The method was demonstrated to be suitable for the determination of metaldehyde in fish meat.
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