Scientia Agricultura Sinica ›› 2007, Vol. 40 ›› Issue (5): 1033-1041 .doi: 10.3864/j.issn.0578-1752.at-2006-7272

• ANIMAL SCIENCE·VETERINARY SCIENCERE·SOURCE INSECT • Previous Articles     Next Articles

Confirmation of fluoroquinolone residues in milk by liquid chromatography-tandem mass spectrometry

  

  1. 华南农业大学兽医学院/广东省兽药研制与安全评价重点实验室
  • Received:2006-03-06 Revised:2006-12-10 Online:2007-05-10 Published:2007-05-10

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Abstract: A confirmation method is developed for determination of 10 fluoroquinolones (FQs), marbofloxacin(MAR), norfloxacin (NOR), ofloxacin (OFL), pefloxacin (PEF), ciprofloxacin (CIP), lomefloxacin (LOM), danofloxacin (DAN), enrofloxacin (ENR), sarafloxacin (SAR) and difloxacin (DIF) in milk using ion-trap-APCI liquid chromatography-tandem mass spectrometry. Milk was precipitated by trichloroacetic acid and acetonitrile and then the extracts were purified onto reverse phase polymer Strata-X cartridges. The determination was achieved by liquid chromatography using an ODS2 analytical column with ion-trap-APCI tandem mass spectrometry. The procedure was validated by spiking 5 FQs (NOR, CIP, PEF, ENR, and SAR) into a blank milk at seven different levels (5.0、10.0、20.0、50.0、100.0、200.0、500.0 ng/mL) and linearity (r2>0.99), accuracy (recovery=48.8%～110.0%), precision (RSD≤18.5%) and sensitivity (LOD=0.2～0.8 ng/mL, LOQ= 1.0～5.0 ng/mL) were checked. The results showed that this method was a high throughputing procedure for confirmation of the FQs residues in milk.

Key words: Fluoroquinolone, Liquid chromatograph-tandem mass spectrometry, Milk, Residue determination

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