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

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• 作者：Mohana Krishna Reddy Mudiam ; Abhishek Chauhan ; Rajeev Jain ; Yogesh Kumar Dhuriya ; Prem Narain Saxena ; Vinay Kumar Khanna
• 关键词：Molecularly imprinted polymer ; Dispersive liquid&ndash ; liquid microextraction ; Injector port silylation ; Gas chromatography&ndash ; tandem mass spectrometry
• 刊名：Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences
• 出版年：15 January, 2014
• 年：2014
• 卷：945-946
• 期：Complete
• 页码：23-30
• 全文大小：1320 K

文摘

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^鈭? and 7.5-2000 ng mL^鈭? 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^鈭? and 1.82 ng mL^鈭? in liver and blood respectively. SRM transition of 271 鈫?#xA0;227 and 271 鈫?#xA0;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.