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土壤中头孢噻呋的高效液相色谱检测方法的建立

Establishment of HPLC for Detection of Ceftiofur in Soil

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【作者】 安博宇徐向月霍美霞马文瑾王涵宇刘振利程古月黄玲利

【Author】 AN Bo-yu;XU Xiang-yue;HUO Mei-xia;MA Wen-jin;WANG Han-yu;LIU Zhen-li;CHENG Gu-yue;HUANG Ling-li;MOA Laboratory for Risk Assessment of Quality and Safety of Livestock and Poultry Products (HZAU);National Reference Laboratory of Veterinary Drug Residues (HZAU) and MOA Key Laboratory for Detection of Veterinary Drug Residues,College of Veterinary Medicine HZAU;

【通讯作者】 程古月;黄玲利;

【机构】 华中农业大学农业部畜禽产品质量安全风险评估实验室华中农业大学国家兽药残留基准实验室(HZAU)农业部食品兽药残留检测重点实验室华中农业大学动物医学院

【摘要】 兽用抗菌药物的大量使用后进入环境后的行为、对环境的污染以及环境耐药基因的诱导现象逐渐受到人们的重视。建立了一种以高效液相色谱(HPLC)检测四种不同类型土壤中兽用抗生素头孢噻呋的方法,为今后此类药物环境行为研究提供方法学借鉴。使用硼酸缓冲液(pH=9)简单提取两次,Waters Oasis HLB固相萃取小柱富集浓缩药物之后,氮吹干,初始流动相复溶,HPLC检测。流动相为0.1%三氟乙酸和乙腈,梯度洗脱之后经过Waters 2998二极管阵列检测器(PDA)进行定量分析。该方法在四种土壤中的加标回收率为70.8%~85.6%,检测限为30μg/kg,定量限为50μg/kg,日内变异系数范围为3.8%~9.8%,日间变异系数范围为4.1%~10.6%。结果表明,本方法高效、稳定、特异性好,可以用于不同类型土壤中头孢噻呋的检测。

【Abstract】 After the behavior and fate in the environment, environmental pollution and the induction of environmental resistance genes have gradually attracted people’ s attention. In this study,a method for the determination of ceftiofur in four different types of soil by high-performance liquid chromatography( HPLC) was established to provide a methodological reference for future research on the environmental behavior of such drugs.Simple extraction was performed twice with boric acid buffer( p H = 9),and the drug was concentrated using a Waters Oasis HLB solid-phase extraction cartridge,and then dried under nitrogen,and the initial mobile phase was reconstituted for HPLC detection. The mobile phase was eluted with a gradient of 0. 1% trifluoroacetic acid and acetonitrile,and then quantitatively analyzed by a Waters 2998 diode array detector( PDA). The recovery rate of the method in four kinds of soil was 70. 8% ~ 85. 6%,the LOD was 30 μg/kg,the LOQ was 50 μg/kg.The intra-day coefficient of variation ranges from 3. 8% ~ 9. 8%,and the inter-day coefficient of variation ranges from 4. 1% to 10. 6%. The results show that the method is efficient,stable and specific,and can be used to detect ceftiofur in different types of soil.

【关键词】 头孢噻呋环境高效液相色谱土壤
【Key words】 ceftiofurenvironmentHPLCsoil
【基金】 国家重点研发计划课题“抗菌药物代谢转归及环境微生态风险评估”(2018YFD0500301)
  • 【文献出处】 中国兽药杂志 ,Chinese Journal of Veterinary Drug , 编辑部邮箱 ,2021年02期
  • 【分类号】X833;O657.72
  • 【下载频次】138
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