液相色谱-串联质谱法检测饲料中洛美沙星、培氟沙星、氧氟沙星、诺氟沙星残留
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摘要
目的建立一种可同时检测饲料中4种氟喹诺酮类药物残留的液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS)检测分析方法。方法试样用磷酸盐缓冲液和乙腈混合进行提取, MCX固相萃取柱净化,以甲醇-0.1%甲酸水溶液为流动相, LC-MS/MS法检测,同时定性、定量测定4种氟喹诺酮类抗生素残留。结果 4种氟喹诺酮类抗生素在HypersilGOLDC_(18)色谱柱上分离效果较好,添加的回收率在60.3%～91.0%之间,相对标准偏差在0.87%～5.91%之间(n=6),方法的检测限为2μg/kg,定量限为5μg/kg。结论该方法准确、简便、快速,能满足兽药残留分析的要求,适合测定饲料中4种氟喹诺酮类抗生素残留。
Objective To establish a method for simultaneous determination of 4 fluoroquinolones residues in feed by liquid chromatography-tandem mass spectrometry(LC-MS/MS). Methods The samples were extracted by mixing phosphate buffer and acetonitrile, purified by MCX solid phase extraction column, and detected by LC-MS/MS with methanol-0.1% formic acid solution as mobile phase. Four fluoroquinolone antibiotic residues were determined qualitatively and quantitatively at the same time. Results Four kinds of fluoroquinolones had good separation effects in Hypersil GOLD C_(18) column. The recoveries were 60.3%-91.0%, with the relative standard deviations of 0.87%-5.91%(n=6). The limit of detection of the method was 2 μg/kg and the limit of quantitation was5 μg/kg. Conclusion The method is accurate, simple and rapid, and can meet the requirements of veterinary drug residue analysis, which is suitable for the determination of four fluoroquinolone antibiotics residues in feed.
Objective To establish a method for simultaneous determination of 4 fluoroquinolones residues in feed by liquid chromatography-tandem mass spectrometry(LC-MS/MS). Methods The samples were extracted by mixing phosphate buffer and acetonitrile, purified by MCX solid phase extraction column, and detected by LC-MS/MS with methanol-0.1% formic acid solution as mobile phase. Four fluoroquinolone antibiotic residues were determined qualitatively and quantitatively at the same time. Results Four kinds of fluoroquinolones had good separation effects in Hypersil GOLD C_(18) column. The recoveries were 60.3%-91.0%, with the relative standard deviations of 0.87%-5.91%(n=6). The limit of detection of the method was 2 μg/kg and the limit of quantitation was5 μg/kg. Conclusion The method is accurate, simple and rapid, and can meet the requirements of veterinary drug residue analysis, which is suitable for the determination of four fluoroquinolone antibiotics residues in feed.
引文
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[8]黄晓蓉,郑晶,李寿崧,等.鳗鱼及其制品中喹诺酮类药物残留的微生物快速检测方法[J].淡水渔业,2005,35(4):3-6.Huang XR,Zheng J,Li SS,et al.Rapid detection of quinolone residues in eels and their products by microorganism[J].Freshwater Fish,2005,35(4):3-6.
[9]李雅丽.喹诺酮类兽药残留的酶联免疫检测方法的研究与建立[D].无锡:江南大学,2008.Li YL.Study and establishment of enzyme-linked immunosorbent assay for residual quinolones of veterinary drugs[D].Wuxi:Jiangnan University,2008.
[10]李慧,祁克宗,邵黎,等.高效毛细管电泳用于饲料中5种氟喹诺酮类药物的同时测定[J].中国饲料,2009,(20):33-37.Li H,Qi KZ,Shao L,et al.Simultaneous determination of five fluoroquinolones in feed by high performance capillary electrophoresis[J].China Feed,2009,(20):33-37.
[11]柯庆青,李诗言,贝亦江,等.HPLC-Q-TOF/MS法同时测定渔用饲料中磺胺类和喹诺酮类药物残留[J].浙江农业科学,2019,(1):129-133.Ke QQ,Li SY,Bai YJ,et al.Simultaneous determination of sulfonamides and quinolones residues in fishery feed by HPLC-Q-TOF/MS[J].Zhejiang Agric Sci,2019,(1):129-133.
[12]岳振峰,谢丽琪,陈小霞,等.牛奶中16种喹诺酮类药物残留量的效液相色谱-串联质谱法测定[J].分析测试学报,2008,27(3):240-243.Yue ZF,Xie LQ,Chen XX,et al.Determination of 16 quinolone residues in milk by high performance liquid chromatography-tandem mass spectrometry[J].J Instrum Anal,2008,27(3):240-243.
[13]彭丽,吴宁鹏,张发旺,等.液相色谱-串联质谱法测定饲料中磺胺类和喹诺酮类药物的含量[J].中国兽药杂志,2014,48(10):53-59.Peng Li,Wu NP,Zhang FW,et al.Determination of sulfonamides and quinolones in feed by liquid chromatography-tandem mass spectrometry[J].Chin J Vet Med,2014,48(10):53-59.
[14]封家旺,李封赛,顾庆云,等.高效液相色谱-串联质谱法测定饲料中6种氟喹诺酮类兽药残留[J].畜牧与兽医,2015,47(3):101-103.Feng JW,Li FS,Gu QY,et al.Determination of six fluoroquinolone veterinary drug residues in feed by high performance liquid chromatography-tandem mass spectrometry[J].Anim Husb Vet Med,2015,47(3):101-103.
[15]张博华.固相萃取-高效液相色谱联用同时分析环境水体中四种喹诺酮类抗生素[D].泰安:山东农业大学,2016.Zhang BH.Simultaneous analysis of four quinolone antibiotics in environmental water by solid phase extraction coupled with high performance liquid chromatography[D].Tai'an:Shandong Agricultural University,2016.
[16]彭玉芬,蔡杰,蔡勤仁,等.固相萃取/UPLC-MS/MS法检测饲料中18种喹诺酮类药物的研究[J].中国兽药杂志,2016,50(12):51-58.Peng YF,Cai J,Cai QR,et al.Study on the determination of 18quinolones in feed by solid phase extraction/UPLC-MS/MS[J].Chin J Vet Med,2016,50(12):51-58.
[17]易建希.饲料中洛美沙星、培氟沙星、氧氟沙星、诺氟沙星的测定-高效液相色谱法[J].湖南饲料,2018,(2):43-45.Yi JX.Determination of lomefloxacin,pefloxacin,ofloxacin and norfloxacin in feed by high performance liquid chromatography[J].Hunan Feed,2018,(2):43-45.
[2]王金秋,马建民,夏曦,等.超高效液相色谱-串联质谱法同时测定猪肌肉中13种喹诺酮药物残留[J].质谱学报,2014,35(2):185-192.Wang JQ,Ma JM,Xia X,et al.Simultaneous determination of 13quinolone residues in pig muscle by ultra performance liquid chromatography tandem mass spectrometry[J].J Chin Mass Spectrom Soc,2014,35(2):185-192.
[3]张俊丰,陈琳.氟喹诺酮类药物在兽医临床的应用[J].兽药与饲料添加剂,2002,7(5):13-15.Zhang JF,Chen L.Clinical application of fluoroquinolones in veterinary medicine[J].Vet Med Feed Addit,2002,7(5):13-15.
[4]李登赴.饲料与畜禽产品质量安全问题浅析[J].贵州畜牧兽医,2008,32(6):19-21.Li DF.Analysis of the quality and safety of feed and livestock products[J].Guizhou Anim Husb Vet Med,2008,32(6):19-21
[5]中华人民共和国农业部公告第2292号[EB/OL].[2015-9-7].http://www.moa.gov.cn/govpublic/SYJ/201509/t20150907_4819267.htm Announcement No.2292 of the Ministry of Agriculture of the People's Republic of China[EB/OL].[2015-9-7].http://www.moa.gov.cn/govpublic/SYJ/201509/t20150907_4819267.htm
[6]刘媛,谢孟峡,丁岚,等.高效液相色谱同时测定鸡蛋中4种氟喹诺酮类药物残留[J].分析化学,2004,32(3):352-355.Liu Y,Xie MX,Ding L,et al.Simultaneous determination of four fluoroquinolones residues in eggs by high performance liquid chromatography[J].Anal Chem,2004,32(3):352-355.
[7]贾涛.液相色谱-荧光法测定饲料中氟喹诺酮类药物[J].饲料广角,2012,(12):43-46.Jia T.Determination of fluoroquinolones in feeds by high performance liquid chromatography-fluorescence spectrometry[J].Feed China,2012,(12):43-46.
[8]黄晓蓉,郑晶,李寿崧,等.鳗鱼及其制品中喹诺酮类药物残留的微生物快速检测方法[J].淡水渔业,2005,35(4):3-6.Huang XR,Zheng J,Li SS,et al.Rapid detection of quinolone residues in eels and their products by microorganism[J].Freshwater Fish,2005,35(4):3-6.
[9]李雅丽.喹诺酮类兽药残留的酶联免疫检测方法的研究与建立[D].无锡:江南大学,2008.Li YL.Study and establishment of enzyme-linked immunosorbent assay for residual quinolones of veterinary drugs[D].Wuxi:Jiangnan University,2008.
[10]李慧,祁克宗,邵黎,等.高效毛细管电泳用于饲料中5种氟喹诺酮类药物的同时测定[J].中国饲料,2009,(20):33-37.Li H,Qi KZ,Shao L,et al.Simultaneous determination of five fluoroquinolones in feed by high performance capillary electrophoresis[J].China Feed,2009,(20):33-37.
[11]柯庆青,李诗言,贝亦江,等.HPLC-Q-TOF/MS法同时测定渔用饲料中磺胺类和喹诺酮类药物残留[J].浙江农业科学,2019,(1):129-133.Ke QQ,Li SY,Bai YJ,et al.Simultaneous determination of sulfonamides and quinolones residues in fishery feed by HPLC-Q-TOF/MS[J].Zhejiang Agric Sci,2019,(1):129-133.
[12]岳振峰,谢丽琪,陈小霞,等.牛奶中16种喹诺酮类药物残留量的效液相色谱-串联质谱法测定[J].分析测试学报,2008,27(3):240-243.Yue ZF,Xie LQ,Chen XX,et al.Determination of 16 quinolone residues in milk by high performance liquid chromatography-tandem mass spectrometry[J].J Instrum Anal,2008,27(3):240-243.
[13]彭丽,吴宁鹏,张发旺,等.液相色谱-串联质谱法测定饲料中磺胺类和喹诺酮类药物的含量[J].中国兽药杂志,2014,48(10):53-59.Peng Li,Wu NP,Zhang FW,et al.Determination of sulfonamides and quinolones in feed by liquid chromatography-tandem mass spectrometry[J].Chin J Vet Med,2014,48(10):53-59.
[14]封家旺,李封赛,顾庆云,等.高效液相色谱-串联质谱法测定饲料中6种氟喹诺酮类兽药残留[J].畜牧与兽医,2015,47(3):101-103.Feng JW,Li FS,Gu QY,et al.Determination of six fluoroquinolone veterinary drug residues in feed by high performance liquid chromatography-tandem mass spectrometry[J].Anim Husb Vet Med,2015,47(3):101-103.
[15]张博华.固相萃取-高效液相色谱联用同时分析环境水体中四种喹诺酮类抗生素[D].泰安:山东农业大学,2016.Zhang BH.Simultaneous analysis of four quinolone antibiotics in environmental water by solid phase extraction coupled with high performance liquid chromatography[D].Tai'an:Shandong Agricultural University,2016.
[16]彭玉芬,蔡杰,蔡勤仁,等.固相萃取/UPLC-MS/MS法检测饲料中18种喹诺酮类药物的研究[J].中国兽药杂志,2016,50(12):51-58.Peng YF,Cai J,Cai QR,et al.Study on the determination of 18quinolones in feed by solid phase extraction/UPLC-MS/MS[J].Chin J Vet Med,2016,50(12):51-58.
[17]易建希.饲料中洛美沙星、培氟沙星、氧氟沙星、诺氟沙星的测定-高效液相色谱法[J].湖南饲料,2018,(2):43-45.Yi JX.Determination of lomefloxacin,pefloxacin,ofloxacin and norfloxacin in feed by high performance liquid chromatography[J].Hunan Feed,2018,(2):43-45.