Chem. J. Chinese Universities ›› 2013, Vol. 34 ›› Issue (12): 2710.doi: 10.7503/cjcu20130764

• Analytical Chemistry • Previous Articles     Next Articles

Simultaneous Determination of Multi-veterinary Drug Residues in Honey by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry and Multiwalled Carbon Nanotubes Cleaning

CAO Hui1,2, CHEN Xiao-Zhen1, ZHU Yan2, LI Zu-Guang3   

  1. 1. Zhejiang Institute of Quality Inspection Science, Zhejiang Food Safety Key Laboratory, Hangzhou 310013, China;
    2. Department of Chemistry, Zhejiang University, Hangzhou 310028, China;
    3. College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, China
  • Received:2013-08-06 Online:2013-12-10 Published:2013-10-23

Abstract:

A method for determining multi-veterinary drug residues in honey by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) and multiwalled carbon nanotubes cleaning was established. This method enabled the comprehensive screening for 52 drugs including sulfonamides, quinolones, nitroimidazoles and tetracyclines. The samples were diluted by Na2EDTA-Mcllvaine solution(pH=4), the clean-up and proconcentration of the analytes were carried out by solid phase extraction cartridge packed with multi-walled carbon nanotubes(MWCNTs). The target analytes were separated by Waters C18 column with gradient elution using acetonitrile and 0.1%(volum fraction) formate in water as mobile phases. The analytes were detected by tandem quadrupole mass spectrometry after positive electrospray ionization by multiple reaction monitoring(MRM). External standard method with matrix was used to determine the results. The correlation coefficient was greater than 0.99 for each drugs. The limits of quantitation(LOQ) were 1.5—7.5 μg/kg. The mean recoveries at the three spiked levels of 7.5, 25, 50 μg/kg were 67.3%—117.8%. The relative standard deviation(RSD) were 1.9%—17.4%. The results indicated that using multi-walled carbon nanotubes as solid phase extraction adsorbent was efficient for the purification. The simplicity, sensitivity and good precision of the method made it be well suitable for determination of multi-veterinary drug residues in honey.

Key words: Multiwalled carbon nanotubes(MWCNTs), Solid phase extraction, Ultra performance liquid chromatography-tandem mass spectrometry, Residue

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