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超高效液相色谱-串联质谱法同时测定牛奶中38种抗生素残留
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方灵,韦航,黄彪,刘文静,苏德森,吴妙鸿,傅建炜 福建省农业科学院农业质量标准与检测技术研究所 
基金项目:福建省农科院科技创新团队资助项目(STIT2017-1-12);国家农业基础性长期性科技工作农产品质量安全观测监测项目(ZX10S1405)
中文摘要:建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定牛奶中5类(磺胺类、喹诺酮类、四环素类、氯霉素类和大环内酯类)38种抗生素的分析方法。牛奶样品以0.5%(体积分数)甲酸乙腈提取,利用Oasis PRiME HLB固相萃取小柱进行净化,经Acquity UPLC HSS T3柱(100 mm×2.1 mm i.d.,1.8 μm)分离,采用电喷雾离子源,多反应监测模式(MRM)进行定性定量分析。结果表明,38种抗生素在各自线性范围内呈良好的线性关系,相关系数(r2)均大于0.99,定量下限为0.10~1.0 μg/kg;在1.0、5.0、10.0 μg/kg加标水平下,平均回收率为70.7%~ 94.9%,相对标准偏差(RSD,n=6)为4.0%~ 9.4%。该方法操作简单、灵敏度高、重现性好,适用于牛奶中多种抗生素残留的监测要求。
中文关键词:牛奶  抗生素  磺胺类  喹诺酮类  四环素类  氯霉素类  大环内酯类  超高效液相色谱-串联质谱(UPLC-MS/MS)
 
Simultaneous Determination of 38 Antibiotics Residues in Milk by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry
Abstract:An analytical method was developed for the simultaneous determination of 38 antibiotics residues in 5 classes of drugs,including sulfonamides,quinolones,tetracyclines,chloramphenicols and macrolides in milk by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted with acetonitrile containing 0.5%(by volume) formic acid,and cleaned up with an Oasis PRiME HLB solid phase extraction column.The target components were separated using an Acquity UPLC HSS T3 column(100 mm×2.1 mm i.d.,1.8 μm),then identified and quantified by UPLC-MS/MS with electrospray ion source(ESI) under multi-reaction ion monitoring(MRM) mode.Results showed that 38 antibiotics had good linear relationships in their respective linear ranges with correlation coefficients(r2) higher than 0.99.The limits of quantitation for 38 antibiotics were between 0.10 μg/kg and 1.0 μg/kg.Average recoveries for 38 antibiotics in milk at spiked levels of 1.0,5.0,10.0 μg/kg ranged from 70.7%to 94.9%,with relative standard deviations(RSD,n=6) of 4.0%-9.4%.With the advantages of easy operation,high sensitivity and good reproducibility,the method was applicable for the determination of antibiotics residues in milk.
Key Words:milk  antibiotics  sulfonamides  quinolones  tetracyclines  chloramphenicols  macrolides  ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
引用本文:方灵,韦航,黄彪,刘文静,苏德森,吴妙鸿,傅建炜.超高效液相色谱-串联质谱法同时测定牛奶中38种抗生素残留[J].分析测试学报,2019,(6):681-676.
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