摘要

Non-aqueous capillary electrophoresis-mass spectrometry (NACE-MS) was developed for trace analyses of beta-agonists (i.e. clenbuterol, salbutamol and terbutaline) in pork. The NACE was in 18 mm ammonium acetate in methanol-acetonitrile-glacial acetic acid (66:33:1, v/v/v) using a voltage of 28 kV. The hyphenation of CE with a time-of-flight MS was performed by electrospray ionization interface employing 5 mm ammonium acetate in methanol-water (80:20, v/v) as the sheath liquid at a flow rate of 2 mu L/min. Method sensitivity was enhanced by a co-injection technique (combination of hydrodynamic and electrokinetic injection) using a pressure of 50 mbar and a voltage of 10 kV for 12 s. The method was validated in comparison with HPLC-MS-MS. The NACE-MS procedure provided excellent detection limits of 0.3 ppb for all analytes. Method linearity was good (r(2)>0.999, in a range of 0.8-1000 ppb for all analytes). Precision showed %RSDs of <17.7%. Sample pre-treatment was carried out by solid-phase extraction using mixed mode reversed phase/cation exchange cartridges yielding recoveries between 69 and 80%. The NACE-MS could be successfully used for the analysis of beta-agonists in pork samples and results showed no statistical differences from the values reported by the Ministry of Public Health, Thailand using HPLC-MS-MS method.

  • 出版日期2010-6