Development and Application of the Dispersive Solid-Phase Extraction Method Based on Molecular Imprinted Polymers for Removal of Matrix Components of Bivalve Shellfish Extracts in the GC–MS/MS Analysis of Amide/Dinitroaniline/Substituted Urea Herbicides

TLDR: A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation method coupled with gas chromatography-tandem mass spectrometry has been developed for the simultaneous analysis of amide/dinitroaniline/substituted urea herbicides in bivalve shellfish samples.

Abstract: A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation method coupled with gas chromatography–tandem mass spectrometry has been developed for the simultaneous analysis of amide/dinitroaniline/substituted urea herbicides in bivalve shellfish samples. A molecularly imprinted polymer (MIP) synthesized through bulk polymerization exhibited strong group–selective interactions with pigments, including β-carotene, chlorophyll A, and fucoxanthin, in bivalve shellfish extracts. Afterward, a modified QuEChERS method based on MIPs and primary and secondary amines was established to effectively remove matrix components in bivalve shellfish samples. Under the optimal conditions, good linearities were obtained in all of the analytes with R2 larger than 0.9995. Limits of quantification were in the range of 0.03–8.88 μg kg−1, respectively. The recoveries of all of the herbicides spiked at three concentrations of 10, 25, and 50 μg kg−1 in blank bivalve shellfish samples ranged from 81 to 109% with intra-day and inter-day relative standard deviations less than 8%, respectively. Results demonstrated that the proposed QuEChERS method coupled with GC–MS/MS was applied successfully to simultaneously determine 26 amide/dinitroaniline/substituted urea herbicides in bivalve shellfish.