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当前位置: 首页 > 文章 > 固相萃取-超高效液相色谱-串联质谱法同时测定动物源性食品中多种兽药残留 食品科学 2017 (12) 266-272
Position: Home > Articles > Simultaneous Determination of Multi-Veterinary Drug Residues in Animal-Origin Food by Solid Phase Extraction Coupled with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry FOOD SCIENCE 2017 (12) 266-272

固相萃取-超高效液相色谱-串联质谱法同时测定动物源性食品中多种兽药残留

作  者：
郝杰;姜洁;余建龙;路勇;毛婷;孙晓冬;杨丽梅
单  位：
北京市食品安全监控和风险评估中心;沃特世科技有限公司
关键词：
固相萃取;超高效液相色谱-串联质谱法;兽药多残留;动物源性食品
摘  要：
利用通过固相萃取法结合超高效液相色谱-串联质谱法建立同时检测猪肉、鱼、虾等动物源性食品中磺胺类、喹诺酮类、糖皮质激素类、大环内酯类、β-受体激动剂类、类固醇激素类、四环素类、青霉素类、氯霉素类、头孢菌素类10大类72种兽药残留的分析方法。样品经80%乙腈溶液提取,直接通过不经活化的Prime HLB固相萃取柱进行净化。使用C_(18)色谱柱分离,电喷雾离子源分段多反应监测扫描模式检测,外标法定量。72种兽药定量限为0.5~5μg/kg,各基质中回收率在75.6%~122.3%之间,相对标准偏差为0.6%~10.7%。本方法极大地提高了多残留兽药的检测效率,适用于食品安全突发事件应急处置中多残留兽药的快速分析。
译  名：
Simultaneous Determination of Multi-Veterinary Drug Residues in Animal-Origin Food by Solid Phase Extraction Coupled with Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
作  者：
HAO Jie;JIANG Jie;YU Jianlong;LU Yong;MAO Ting;SUN Xiaodong;YANG Limei;Beijing Municipal Center for Food Safety Monitoring;Waters Technology Co.Ltd.;
关键词：
solid phase extraction;;ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS);;veterinary drug multiresidues;;animal-derived food
摘  要：
An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with solid phase microextraction method was established for the simultaneous determination of 72 veterinary drugs including sulfanilamide, quinolone, glucocorticoid, macrolides, beta-agonist, steroid hormone, tetracycline, penicillin, chloramphenicol and betalactam in pork, fish and shrimp samples. Samples were extracted by 80%(V/V) acetonitrile in water, followed by cleanup of the extracts through a Prime HLB solid phase extraction column directly without activation. Separation was performed on a C18 column and the eluates were detected by multiple reaction monitoring scanning with electronic spray ionization. An external standard method was applied for quantification. The limits of quantitation(LOQ) for 72 veterinary drugs were in the range of 0.5 to 5 μg/kg. Recoveries from different food matrices were from 75.6% to 122.3% with relative standard deviations between 0.6% and 10.7%. This method was significantly efficient in the determination of multiple veterinary drugs and suitable for rapid multiresidual analysis of veterinary drugs in handling of food safety emergencies.

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