Molecularly imprinted polymer coupled with dispersive liquid–liquid microextraction and injector port silylation: A novel approach for the determination of 3-phenoxybenzoic acid in complex biological samples using gas chromatography–tandem mass spectromet

• First report on MIP-DLLME-IPS followed by GC–MS/MS analysis for 3-phenoxybenzoic acid.
• Selective extraction of 3-PBA with good linearity with R2 of 0.9963 and 0.9898 in blood and liver, respectively.
• The recovery was found in the range of 83–91%.
• The detection limit of 0.0045 ng mg−1 and 1.82 ng mL−1 in liver and blood, respectively.

A novel analytical approach based on molecularly imprinted solid phase extraction (MISPE) coupled with dispersive liquid–liquid microextraction (DLLME), and injector port silylation (IPS) has been developed for the selective preconcentration, derivatization and analysis of 3-phenoxybenzoic acid (3-PBA) using gas chromatography–tandem mass spectrometry (GC–MS/MS) in complex biological samples such as rat blood and liver. Factors affecting the synthesis of MIP were evaluated and the best monomer and cross-linker were selected based on binding affinity studies. Various parameters of MISPE, DLLME and IPS were optimized for the selective preconcentration and derivatization of 3-PBA. The developed method offers a good linearity over the calibration range of 0.02–2.5 ng mg−1 and 7.5–2000 ng mL−1 for liver and blood respectively. Under optimized conditions, the recovery of 3-PBA in liver and blood samples were found to be in the range of 83–91%. The detection limit was found to be 0.0045 ng mg−1 and 1.82 ng mL−1 in liver and blood respectively. SRM transition of 271 → 227 and 271 → 197 has been selected as quantifier and qualifier transition for 3-PBA derivative. Intra and inter-day precision for five replicates in a day and for five, successive days was found to be less than 8%. The method developed was successfully applied to real samples, i.e. rat blood and tissue for quantitative evaluation of 3-PBA. The analytical approach developed is rapid, economic, simple, eco-friendly and possess immense utility for the analysis of analytes with polar functional groups in complex biological samples by GC–MS/MS.