Chinese Journal of Chromatography

Chinese Journal of Chromatography ›› 2014, Vol. 32 ›› Issue (6): 573-581.DOI: 10.3724/SP.J.1123.2014.02014

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Simultaneous determination of nine β-blockers in porcine tissues by ultra-fast liquid chromatography coupled with quadrupole/linear ion trap mass spectrometry

ZHANG Hongwei1, XU Hui1, GAO Jianguo2, LIANG Chengzhu1, XU Biao1, GENG Juan1, WANG Fengmei1, ZHANG Xiaomei1, CHENG Gang1   

  1. 1. Technical Center of Inspection and Quarantine, Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China;
    2. Qingdao Entry-Exit Inspection and Quarantine Bureau, Qingdao 266001, China
  • Received:2014-02-17 Revised:2014-03-21 Online:2014-06-08 Published:2014-05-22

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Abstract:

A highly sensitive method using ultra-fast liquid chromatography coupled with quadrupole/linear ion trap mass spectrometry (UFLC-Q/Trap MS) was developed to simultaneously screen and confirm nine β-blockers (BBs) in porcine tissues (porcine muscle, liver and kidney). The method was used for trace determination of atenolol, pindolol, acebutolol, metoprolol, carazolol, labetalol, bisoprolol, propranolol and penbutolol. The homogenized tissues were hydrolyzed by β-glucuronidase/aryl sulfatase and extracted with acetonitrile, followed by continuous purification procedures of disperse solid phase extraction (d-SPE) with diatomaceous earth and BondElut cartridge. The ultra-fast chromatographic separation was conducted on a KinetexTM C18-XB column (150 mm×2.1 mm, 2.6 μm) using 0.1% (v/v) formic acid aqueous solution and methanol as mobile phases in gradient elution. The optimized ion transitions were employed in the mixed-mode of scheduled multiple reaction monitoring (sMRM)-information dependent acquisition (IDA)-enhanced product ion (EPI) scan. Qualification analysis was performed through spectra-matching with on-line lab-built MS/MS library. For quantification stable isotope-labelled analogues of the analytes were used as internal standards. As a result, in porcine liver, kidney and muscle, the nine BBs showed good linearity with all the correlation coefficients (r) more than 0.995 in the range of 0.1-20 μg/L. The limits of quantification (LOQ, S/N≥10) were 0.5 μg/kg for all the analytes. The developed method gave average recoveries of 87.5%-111.8% spiked at 0.5, 1.0 and 5.0 μg/kg with the relative standard deviations of 4.0%-12.5%. The proposed method can be used to screen and confirm the nine BBs in a single run, which makes it effective in surveillance and detection of the BBs residues in porcine tissues.

Key words: β-blockers (BBs), porcine tissues, quadrupole/linear ion trap mass spectrometry (Q/Trap MS), residue, ultra-fast liquid chromatography (UFLC)

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