Determination of β-Agonist Residues in Animal-Derived Food by a Liquid Chromatography-Tandem Mass Spectrometric Method Combined with Molecularly Imprinted Stir Bar Sorptive Extraction.

Jiwang Tang,Shengqiang Hu,Liejiang Yuan,Jianxiu Wang,Shuyun Shi

doi:10.1155/2018/9053561

Abstract

A novel clenbuterol molecularly imprinted polymer (MIP)-coated stir bar was prepared and applied to the determination of six β-agonists in animal-derived food. Characterization and various parameters affecting adsorption and desorption behaviours were investigated. The extraction capacities of clenbuterol, salbutamol, ractopamine, mabuterol, brombuterol, and terbutaline for MIP coating were 3.8, 2.9, 3.1, 3.5, 3.2, and 3.3 times higher, respectively, than those of the NIP coating, respectively. The method of MIP-coated SBSE coupled with HPLC-MS/MS was developed. The recoveries in pork and liver samples were 75.8–97.9% with RSD from 2.6 to 5.3%. Limits of detection (LODs) and limits of quantification (LOQs) were 0.05–0.15 μg/kg and 0.10–0.30 μg/kg, respectively. Good linearities were obtained for six β-agonists with correlation coefficients (R 2) higher than 0.994. These results indicated the superiority of the proposed method in the analysis of β-agonists in a complex matrix.

Highlights

E aim of this present work was to prepare an molecularly imprinted polymer (MIP) coating on the glass stir bar and apply it to the selective stir bar sorptive extraction (SBSE) of clenbuterol and its analogue compounds. e preparation parameters and extraction conditions, which affected the extraction performance of the stir bar, were studied in detail
E extraction capacity and selectivity of the clenbuterol MIP-coated stir bar were evaluated. en, a method of determination of structural-related β-agonists by MIP-SBSE followed by HPLC-MS/MS was developed. e proposed method was successfully applied to the analysis of β-agonists in animal-derived food
Soaking of the glass bar in alkaline solution is performed in order to expose the maximum number of silanol groups on the surface to promote silylation with the silane coupling agent. us, double bonds were present in the molecular structure, forming an active site for the MIP coating

Summary

Introduction

E aim of this present work was to prepare an MIP coating on the glass stir bar and apply it to the selective SBSE of clenbuterol and its analogue compounds. e preparation parameters and extraction conditions, which affected the extraction performance of the stir bar, were studied in detail. E aim of this present work was to prepare an MIP coating on the glass stir bar and apply it to the selective SBSE of clenbuterol and its analogue compounds. E extraction capacity and selectivity of the clenbuterol MIP-coated stir bar were evaluated. En, a method of determination of structural-related β-agonists by MIP-SBSE followed by HPLC-MS/MS was developed. E silane coupling agent KH-570 was purchased from Sinopharm Chemical Reagent Co. Ltd. HPLC-grade methanol, toluene, and acetonitrile were purchased from Merck (Darmstadt, Germany). E coating surface of the stir bar was characterized by a VEGA3 scanning electron microscope (TESCAN, Czech Republic), and the composition of the coating was investigated using a Fourier transform infrared (FT-IR) spectrometer (Nicolet iS5, ermo, USA). Measurements were taken using a TSQ Quantum Ultra triple quadrupole mass spectrometer ( ermo, USA) equipped with an electrospray ion source and coupled with an Accela liquid chromatography ( ermo, USA), equipped with a Hypersil GOLD (100 mm × 2.1 mm i. d., 3 μm) column

Methods

Results

Conclusion