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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 |
| 安博宇,徐向月,霍美霞,马文瑾,刘振利,王涵宇,程古月,黄玲利 |
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| (华中农业大学农业部畜禽产品质量安全风险评估实验室(武汉）;华中农业大学农业部畜禽产品质量安全风险评估实验室(武汉）;华中农业大学国家兽药残留基准实验室HZAU) |
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| 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30 μg/kg，定量限为50 μg/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。 |
| 关键词: 头孢噻呋 环境 高效液相色谱 土壤 |
| DOI： |
| 投稿时间：2020-06-23修订日期：2021-01-13 |
| 基金项目: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) |
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| Establishment of HPLC for detection of ceftiofur in soil |
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| (MOA Laboratory for Risk Assessment of Quality and Safety of Livestock and Poultry Products HZAU) |
| 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 (pH=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. |
| Key words: Ceftiofur Environment HPLC Soil |
