超高效液相色谱-串联质谱法同时测定液态奶中克拉维酸和舒巴坦

doi:10.7506/spkx1002-6630-201316052

食品科学

超高效液相色谱-串联质谱法同时测定液态奶中克拉维酸和舒巴坦

马晓斐，张敬轩，李挥，张翠侠，梁天佐，张岩

1.河北省食品质量监督检验研究院，河北石家庄 050091；2.河北医科大学法医学系，河北石家庄 050017

出版日期:2013-08-25 发布日期:2013-09-03

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. 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

摘要/Abstract

摘要：

建立同时测定液态奶中克拉维酸和舒巴坦的超高效液相色谱-串联质谱法。试样通过乙腈沉淀蛋白，经Agilent ZORBAX SB-C18(2.1mm×150mm，3.5μm)色谱柱分离，采用电喷雾电离，多反应监测模式下进行测定。结果表明：克拉维酸和舒巴坦在各自质量浓度范围内线性良好，R2大于0.9990。在低、中、高3个添加水平下，克拉维酸和舒巴坦的平均回收率稳定在77.9%～93.1%之间，相对标准偏差为3.9%～8.8%，检出限分别为2.0μg/kg和5.0μg/kg。该方法操作简便、灵敏度高、回收率和重复性良好，适用于液态奶中克拉维酸和舒巴坦药物残留的测定。

关键词: 液态奶, 超高效液相色谱-串联质谱, 克拉维酸, 舒巴坦

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

马晓斐，张敬轩，李挥，张翠侠，梁天佐，张岩. 超高效液相色谱-串联质谱法同时测定液态奶中克拉维酸和舒巴坦[J]. 食品科学, doi: 10.7506/spkx1002-6630-201316052.

MA Xiao-fei，ZHANG Jing-xuan，LI Hui，ZHANG Cui-xia，LIANG Tian-zuo，ZHANG Yan. Determination of Clavulanic Acid and Sulbactam in Milk by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, doi: 10.7506/spkx1002-6630-201316052.

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超高效液相色谱-串联质谱法同时测定液态奶中克拉维酸和舒巴坦

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

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