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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
【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.
- 【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