Determination of 9 Pyrrolizidine Alkaloids in Animal derived Foods by HPLC-MS/MS

KeyWord:animal derived food  pyrrolizidine alkaloids  solid phase extraction  high performance liquid chromatography-tandem mass spectrometry£¨HPLC-MS/MS£©

Abstract:

      A method of high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was developed for the determination of nine pyrrolizidine alkaloid residues in animal derived foods.Honey,dairy and animal liver samples were dissolved with 0.05 mol/L hydrochloric acid,5% trichloroacetic acid and acetonitrile containing 1% acetic acid,respectively,then enriched and purified with a strong cationic solid phase extraction column(Waters Oasis MCX).The separation was carried out on a Phenomenex Kinetex C18 column(4.6 mm¡Á100 mm,2.6 ¦Ìm) by gradient elution with methanol-0.1% formic acid-5 mmol/L ammonium acetate as mobile phase.The separated compounds were detected in positive electrospray ionization(ESI+) under multiple reaction monitoring(MRM) mode.The calibration curves for 9 alkaloids were linear in the mass concentration range of 0-100 ng/mL with correlation coefficients(r) larger than 0.99.The average recoveries at there spiked levels of 10,20 and 50 ¦Ìg/kg ranged from 71.0% to 103%,with relative standard deviations(RSD) of 3.0%-9.8%.The limits of detection and limits of quantitation(LOQs) of the method were 3 ¦Ìg/kg and 10 ¦Ìg/kg,respectively.The method is simple,rapid and accurate,and is suitable for the simultaneous determination of pyrrolizidine alkaloids in animal derived foods.