摘要
建立了配合饲料中16种头孢类药物(头孢氨苄、头孢拉定、头孢唑林、头孢哌酮、头孢乙腈、头孢匹林、头孢洛宁、头孢喹肟、头孢噻肟、头孢噻呋、头孢噻吩、头孢羟氨苄、头孢呋辛、头孢他定、头孢克洛、头孢丙烯)含量的液相色谱-串联质谱测定方法。配合饲料样品中头孢类药物用乙腈-水(40∶60)溶液提取,离心,上清液经0. 1%甲酸稀释后进行液相色谱-串联质谱分析。采用Acquity BEH C18色谱柱,以0. 1%甲酸溶液-甲醇作为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,基质校准外标法定量。结果表明,16种头孢类药物在一定质量浓度范围内均呈良好的线性关系,相关系数(r2)均大于0. 999;方法检出限为1. 5～15μg/kg,定量下限为5. 0～50μg/kg。阴性配合饲料样品的加标回收率为88. 4%～93. 6%,相对标准偏差(RSD)为0. 8%～4. 7%。该方法简单快速,准确度和精密度较好,能满足配合饲料样品中头孢类药物的检测需要。
A simple,sensitive and reliable analytical method was developed for the simultaneous determination of 16 cephalosporins in formulated feeds by ultra high performance liquid chromatography-positive electrospray ionization tandem mass spectrometry.Samples were extracted with acetonitrile-water(40∶60)solution,and directly diluted using 0.1%formic acid solution after centrifugation,then analyzed by LC-MS/MS.The samples were separated on an Acquity UPLC BEH C 18 column with a mixture of 0.1%formic acid solution and methanol as mobile phase by gradient elution,and detected in multiple reaction monitoring mode.The matrix-matched external standard method was applied for the quantitative analysis.There are good linear relationships for sixteen cephalosporins in the certain concentration ranges with their correlation coefficients more than 0.999.The limits of detection for sixteen cephalosporins were in the range of 1.5-15μg/kg,and the limits of quantitation were 5.0-50μg/kg.The recoveries for the analytes in feeds at spiked levels of 10-2 500μg/kg were in the range of 88.4%-93.6%,with relative standard deviations of 0.8%-4.7%.The method is suitable for the determination of sixteen cephalosporins in formulated feeds due to its simplicity and reliability.
作者
张艳
吴银良
ZHANG Yan;WU Yin-liang(The Ningbo Academy of Agricultural Sciences,Ningbo 315040,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2018年第11期1365-1370,共6页
Journal of Instrumental Analysis
基金
宁波市农业资助项目(2016C51036)
关键词
配合饲料
头孢菌素类药物
液相色谱-串联质谱法
含量
formulated feeds
cephalosporins
liquid chromatography with tandem mass spectrometry
concentration
