Determination of 42 Herbicides Residues in Shellfish Using Captiva EMR-Lipid Clean-up in Combination with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry
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(1.Binzhou Testing Center, Binzhou 256600, Shandong;2.Shandong Provincial Engineering and Technology Research Center for Wild Plant Resources Development and Application of Yellow River Delta, College of Biological and Environmental Engineering, Binzhou University,Binzhou 256600, Shandong)

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    Abstract:

    Based on enhanced matrix removal lipid column (Captiva EMR-Lipid) purified, a method was developed for determination of 42 kinds of triazine, amide and sulfonylurea herbicides residues in shellfish by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). After optimizing the pretreatment and chromatographic conditions, acetonitrile, Captiva EMR-Lipid column were used as the extraction solvents and purification agents, respectively. The separation of 42 analytes was performed on a Shim-pack GIST C18-AQ column (100 mm × 2.1 mm, 1.9 μm) with gradient elution. The MS/MS detection was performed with electrospray ionization in positive ion mode and multiple reaction monitoring mode. The 42 analytes showed great linear relationships in the range of 0.2-20 μg/L with correlation coefficients (R2) all above 0.992. The limits of detection (LODs) were 0.2-0.4 μg/kg and the limits of quantitation (LOQs) were 0.5-1.0 μg/kg. The average recoveries of analytes varied from 61.0% to 110.3%, and the relative standard deviations (RSDs) were between 0.1% and 17.4%. Using the established determination method, 23 shellfish samples were detected, and 5 kinds of herbicides residues were detected. The method was simple, rapid, high accurate and sensitive, which was suitable for the simultaneous determination of 42 kinds of herbicides residues in shellfish.

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  • Received:January 27,2022
  • Online: February 24,2023
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