Citation: ZHENG Ling, WU Yujie, ZHAO Yongfeng, LI Lihua, MA Yanjuan. Simultaneous determination of 18β-agonist residues in feed using QuEChERS sample preparation and high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(8): 867-873. doi: 10.3724/SP.J.1123.2014.03029 shu

Simultaneous determination of 18β-agonist residues in feed using QuEChERS sample preparation and high performance liquid chromatography-tandem mass spectrometry

1.
Guangxi Entry-Exit Inspection and Quarantine Bureau, Nanning 530021, China

Corresponding author: WU Yujie,
Received Date: 19 March 2014
Available Online: 22 April 2014
Fund Project: 广西科技厅2012重大专项课题(桂科重:1222003-2-1). (桂科重:1222003-2-1)

A multi-residue method was developed for the simultaneous determination of 18 β-agonist residues (clenbuterol, ractopamine, penbutolol, tulobuterol, etc) in feed by using QuEChERS sample preparation and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The feed samples were dispersed by water, then the analytes were extracted with acetonitrile containing 4%(v/v) ammonia and cleaned up by QuEChERS method with 25 mg octadecylsilyl (C₁₈) and 50 mg primary secondary amine (PSA) adsorbents. The separation of compounds was carried on an Agilent ZORBAX Eclipse XDB-C₁₈ column (50 mm×4.6 mm, 1.8 μm) by a gradient elution using methanol-0.1%(v/v) formic acid aqueous solution as mobile phase. The analytes were detected by tandem mass spectrometry under multiple reaction monitoring (MRM) mode with positive electrospray ionization (ESI⁺) and quantified by the matrix-matched external standard method. The results showed that the calibration curves of the 18 β-agonists were linear in the range of 5-200 μg/L with correlation coefficients of 0.9912-0.9995. The average recoveries of the 18 analytes at three spiked levels of 0.05, 0.1 and 0.5 mg/kg ranged from 78.4% to 107.1% with the relative standard deviations (RSDs) of 3.5%-12.3%. The limit of quantification (LOQ, S/N≥10) was 0.05 mg/kg for each analyte . The developed method is simple and sensitive, and can be applied as a screen and confirmatory method for the analysis of β-agonists in feed.
- QuEChERS,
- high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS),
- β -agonists,
- feed
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