高效液相色谱-串联质谱法同时测定水产品中四环素类抗生素及盐酸克伦特罗药物残留量  被引量:8

Simultaneous determination of tetracycline and clenbuterol residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry

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作  者:李小玲[1,2] 万译文[1,2] 邓克国[1] 

机构地区:[1]农业部渔业产品质量监督检验测试中心(长沙),长沙410153 [2]湖南省水产科学研究所,长沙410153

出  处:《分析试验室》2013年第9期86-89,共4页Chinese Journal of Analysis Laboratory

摘  要:建立了水产品中四环素类抗生素和盐酸克伦特罗药物残留量同时测定的高效液相色谱一串联质谱方法。样品选择NH4Ac缓冲液提取,用正己烷脱脂,PCx固相萃取柱净化,采用HPLC—MS/MS选择反应监测正离子模式测定进行定性、定量分析。四环素类抗生素和盐酸克伦特罗药物的检出限为0.25μg/kg,定量限为0.5μg/kg,RSD为1.9%-12%(n=6),加标回收率达到64.3%~100.6%。该方法在水产品中四环素类抗生素和盐酸克伦特罗的残留测定中具有很好的应用前景。An analytical method for the determination of tetracycline and clenbuterol residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established. The sample was extracted with ammonium acetate buffer, defatted-up by hexane, and cleaned up using mixed-mode cation exchange solid-phase extraction cartridges (PCX). The mass spectrometer was operated in the positive ion mode using selected reaction monitoring for the qualitative and quantitative analysis. The detection limits of this method for tetracyclines and clenbuterol residues were 0. 25μg/kg, and the limits of quantification were 0.5 μg/kg. The relative standard deviations ranged from 1.9% to 12% (n =6) and the recoveries were from 64.3% to 100.6%. The method proposed by this paper possesses high reproducibility and selectivity. It is expected that it could be applied to the determination of the tetracycline and clenbuterol residues in aquatic products.

关 键 词:高效液相色谱-串联质谱法 四环素类抗生素 盐酸克伦特罗 水产品 

分 类 号:O657.63[理学—分析化学]

 

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