摘要
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。
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 monitoring （dMRM）. The result indicated that the limits of detection （LOD） were 1.0 μg/kg-1 and the limits of quantitation （LOQ） were 2.0 txg/kg. The linear correlation coefficients were more than 0. 9960. The average recoveries ranged from 77% to 115% with RSDs less than 10%. This method was suitable for the identification and quantification of multi-component veterinary drugs in feeds due to its simplicity, high sensitivity and lower matrix effect.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2014年第2期233-238,共6页
Chinese Journal of Analytical Chemistry
基金
国家质检总局科技计划(No.2012QK029)资助项目
关键词
超高效液相色谱-串联质谱
稳定同位素内标
动态多反应监测
禁用兽药
饲料
Ultra high performance liquid chromatography-tandem mass spectrometry
Stable isotope-labeled internal standard
Dynamic multiple reaction ion monitoring
Banned veterinary drugs
Feed
