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LIQUID CHROMATOGRAPHY

Determination of β2-Agonists in Porcine Urine by Molecularly Imprinted Solid Phase Extraction Followed Ultra-Performance Liquid Chromatography–Tandem Mass Spectrometry Detection

, , , , , , & show all
Pages 734-744 | Received 21 Aug 2012, Accepted 26 Sep 2012, Published online: 01 Mar 2013
 

Abstract

A novel, sensitive, and robust method has been developed to detect 9 β2-agonists in porcine urine to monitor illegal use of β2-agonists in swine rearing. The method based on the molecular imprinted polymer (MIP) rapid extraction followed ultra-performance liquid chromatography coupled tandem mass spectrometry (UPLC-MS/MS) detection. The cleaning efficiency of MIP cartridges was demonstrated by comparing with common ion exchange solid phase extraction. The presented method was validated in accordance with the European Commission Decision 2002/657/EC. The linearity, decision limit (CCα), detection capability (CCβ), recovery, precision, robustness, and stability were studied in detail. CCα and CCβ values were from 0.006 ng/mL to 0.03 ng/mL and from 0.02 ng/mL to 0.08 ng/mL, respectively. The mean recoveries and repeatability varied from 68.8% to 94.2% and from 2.8% to 10.1%. The proposed method was applied to test 170 porcine urine samples from the Shaanxi province in China and two urine samples were confirmed as clenbuterol positive and the concentrations of clenbuterol in positive urine samples were about 0.08 ng/mL and 0.1 ng/mL, respectively. The developed method was demonstrated to be more sensitive and robust for the determination of 9 β2-agonists in porcine urine. The method was proven to be simple and easy in operation with high selectivity and good reproducibility.

Acknowledgments

We would like to acknowledge the Special Fund for Agricultural Research (Contract No. 201203088) for financial support.

Notes

Note. RSD is relative standard deviation.

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