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Determination of Clavulanic Acid and Sulbactam in Milk by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

MA Xiao-fei,ZHANG Jing-xuan,LI Hui,ZHANG Cui-xia,LIANG Tian-zuo,ZHANG Yan   

  1. 1. Hebei Institute of Food Quality Supervision Inspection and Research, Shijiazhuang 050091, China;
    2. Department of Forensic Medicine, Hebei Medical University, Shijiazhuang 050017, China
  • Online:2013-08-25 Published:2013-09-03

Abstract:

An integrated analytical method based on ultra-performance liquid chromatography coupled with tandem mass
spectrometry (UPLC-MS-MS) has been developed for the simultaneous determination of clavulanic acid and sulbactam in
milk. Samples were deproteinized by acetonitrile. Mass spectral data were acquired in electrospray ion (ESI) mode using
multiple reaction monitoring (MRM) scan after chromatographic separation on Agilent ZORBAX SB-C18 (2.1 mm ×
150 mm , 3.5 μm) column. An excellent linear relationship in their respective concentration ranges was observed for the
two analytes with a correlation coefficient larger than 0.9990. The average recoveries from spiked blank samples ranged
from 77.9% to 93.1% with relative standard deviation (RSD) between 3.9% and 8.8%. The limits of detection (LOD) for
clavulanic acid and sulbactam were 2.0 μg/kg and 5.0 μg/kg, respectively. With the advantages of convenience, sensitivity,
good recovery and repeatability, the method was suitable for the detection of clavulanic acid and sulbactam in milk.

Key words: milk, ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS-MS), clavulanic acid, sulbactam