稳定同位素稀释超高效液相色谱-串联质谱法测定饲料中24种禁用兽药含量

建立了同时定性与定量分析动物饲料种24中禁用药物的超高效液相色谱串联质谱（UHPLC-MS/MS）分析方法。样品经Na2HPO4与饱和NaCl溶液共同盐析,乙腈提取,混合阳离子交换固相萃取柱（PCX）净化,乙腈和0.3%甲酸溶液梯度洗脱,经BEH C18色谱柱分离,串联四级杆质谱动态多反应监测正离子模式监测,稳定同位素标记内标法定量。在最佳实验条件下,24种禁用兽药在各自的线性范围内线性关系良好,相关系数（r）均大于0.9960,检出限为1.0μg/kg,定量限为2.0μg/kg,加标回收率在77%~115%之间,相对标准偏差小于10%。本方法的样品前处理过程简单,净化效果好,有效解决了基质效...

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Bibliographic Details
Published in分析化学 Vol. 42; no. 2; pp. 233 - 238
Main Author 周鹏 林钦 黄红霞 杨旺火 戴明 刘飞 王瑛
Format Journal Article
LanguageChinese
Published 南京理工大学化工学院,南京210094 2014
国家加工食品质量监督检验中心(福州),福州350002%国家加工食品质量监督检验中心(福州),福州,350002%南京理工大学化工学院,南京,210094
Subjects
动态多反应监测
禁用兽药
稳定同位素内标
超高效液相色谱-串联质谱
饲料
超高效液相色谱-串联质谱
Banned veterinary drugs
Ultra high performance liquid chromatography-tandem mass spectrometry
动态多反应监测
禁用兽药
饲料
稳定同位素内标
Stable isotope-labeled internal standard
Dynamic multiple reaction ion monitoring
Feed
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ISSN0253-3820
DOI10.3724/SP.J.1096.2014.30957

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Summary:建立了同时定性与定量分析动物饲料种24中禁用药物的超高效液相色谱串联质谱（UHPLC-MS/MS）分析方法。样品经Na2HPO4与饱和NaCl溶液共同盐析,乙腈提取,混合阳离子交换固相萃取柱（PCX）净化,乙腈和0.3%甲酸溶液梯度洗脱,经BEH C18色谱柱分离,串联四级杆质谱动态多反应监测正离子模式监测,稳定同位素标记内标法定量。在最佳实验条件下,24种禁用兽药在各自的线性范围内线性关系良好,相关系数（r）均大于0.9960,检出限为1.0μg/kg,定量限为2.0μg/kg,加标回收率在77%~115%之间,相对标准偏差小于10%。本方法的样品前处理过程简单,净化效果好,有效解决了基质效应问题,灵敏度高,适用于各种饲料中多组分禁用兽药的快速定性与定量分析。
Bibliography:ZHOU Peng, LIN Qin, HUANG Hong-Xia, YANG Wang-Huo, DAI Ming, LIU Fei, WANG Ying1 （ School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China） z（ National Center for Quality Supervision and Inspection of Processed Foods （FuZhou） , Fuzhou 350002, China）
Ultra high performance liquid chromatography-tandem mass spectrometry; Stable isotope-labeled internal standard; Dynamic multiple reaction ion monitoring; Banned veterinary drugs; Feed
A method based on ultra high performance liquid chromatography-tandem mass spectrometry （UHPLC-MS/MS） was developed for the determination of 24 banned veterinary drugs in feed. The sample was extracted with Na2HPO4 ,Saturated NaC1 solution and acetonitrile, and then cleaned up by PCX solid-phase extraction column. The target analytes were separated on BEH Cts column using gradient elution of acetonitrile and 0.3% formic acid, detected by MS/MS system under positive electro-spray ionization（ ESI~） mode with dynamic multiple reaction ion monit
ISSN:0253-3820
DOI:10.3724/SP.J.1096.2014.30957