title: 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 spectrometry.
abstract: 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 0.02-2.5ngmg(-1) and 7.5-2000ngmL(-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 0.0045ngmg(-1) and 1.82ngmL(-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.
authors: Academy of Scientific and Innovative Research, Council of Scientific & Industrial Research, PO Box-80, MG Marg, Lucknow 226001, India; Analytical Chemistry Section, CSIR-Indian Institute of Toxicology Research, PO Box-80, MG Marg, Lucknow 226001, India. Electronic address: mohanitrc@gmail.com.
authors: Mohana Krishna Reddy
authors: MK
authors: Mudiam
authors: Academy of Scientific and Innovative Research, Council of Scientific & Industrial Research, PO Box-80, MG Marg, Lucknow 226001, India; Analytical Chemistry Section, CSIR-Indian Institute of Toxicology Research, PO Box-80, MG Marg, Lucknow 226001, India.
authors: Abhishek
authors: A
authors: Chauhan
authors: Analytical Chemistry Section, CSIR-Indian Institute of Toxicology Research, PO Box-80, MG Marg, Lucknow 226001, India.
authors: Rajeev
authors: R
authors: Jain
authors: Developmental Toxicology, CSIR-Indian Institute of Toxicology Research, PO Box-80, MG Marg, Lucknow 226001, India.
authors: Yogesh Kumar
authors: YK
authors: Dhuriya
authors: Academy of Scientific and Innovative Research, Council of Scientific & Industrial Research, PO Box-80, MG Marg, Lucknow 226001, India.
authors: Prem Narain
authors: PN
authors: Saxena
authors: Developmental Toxicology, CSIR-Indian Institute of Toxicology Research, PO Box-80, MG Marg, Lucknow 226001, India.
authors: Vinay Kumar
authors: VK
authors: Khanna
mesh_terms: D000818:Animals; D001565:Benzoates / Q000032:analysis* / Q000097:blood*; D008401:Gas Chromatography-Mass Spectrometry / Q000191:economics / Q000379:methods*; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000191:economics / Q000379:methods*; D008099:Liver / Q000737:chemistry*; D054802:Molecular Imprinting; D051381:Rats; D017208:Rats, Wistar; D053719:Tandem Mass Spectrometry / Q000191:economics / Q000379:methods
chemical_list: D001565:Benzoates; C017618:3-phenoxybenzoic acid
keywords: Dispersive liquid–liquid microextraction; Gas chromatography–tandem mass spectrometry; Injector port silylation; Molecularly imprinted polymer