头孢噻呋及去呋喃甲酰基头孢噻呋的四极杆轨道阱串联质谱分析及其在肉鸡体内的残留规律研究

发布时间：2018-05-03 08:53

本文选题：四极杆轨道阱串联质谱(Q-Orbitrap + MS)　；参考：《质谱学报》2017年05期

【摘要】：建立了头孢噻呋及其主要代谢物去呋喃甲酰基头孢噻呋残留的超高效液相色谱-四极杆轨道阱串联质谱(UHPLC-Q-Orbitrap MS)分析方法。选用Kinetex F5 100A色谱柱(50mm×3.0mm×2.6μm)分离,在Q-Exactive高分辨质谱Full MS/dd-MS2扫描模式下采集数据进行定性定量分析。两种目标物在3种基质中相应浓度范围内的线性关系良好,相关系数r2均大于0.990,回收率为83.2%~129.7%,RSD均小于15%。通过对鸡体内头孢噻呋及其代谢物残留规律的分析表明,给药后,鸡胸肉中头孢噻呋和去呋喃甲酰基头孢噻呋均可检出,且消除时间均为12~24h;鸡肝、鸡肾中头孢噻呋可在0.5h内迅速代谢为去呋喃甲酰基头孢噻呋,鸡肝和鸡肾中去呋喃甲酰基头孢噻呋的消除时间分别为48~72h和72~120h。本研究可为保障动物源性食品安全以及鸡体内头孢噻呋最大残留限量标准和休药期的制订提供理论和实践依据。
[Abstract]:A high performance liquid chromatography-quadrupole orbital trap tandem mass spectrometry (UHPLC-Q-Orbitrap) method was developed for the determination of cefotioxime and its main metabolite, defurfuryl cefotaxime. A 50 mm 脳 3.0mm 脳 2.6 渭 m Kinetex F5100A column was used for qualitative and quantitative analysis of the data collected by Q-Exactive high resolution mass spectrometry Full MS/dd-MS2 scanning mode. The linear relationship between the two targets in the corresponding concentration range of the three substrates is good, the correlation coefficient R2 is greater than 0.990, the recovery rate is 83.2 and 129.7% RSD is less than 15%. The results of analysis of cefotaxime and its metabolites in chicken body showed that both cefotioxime and defuranyl cefotioxime could be detected in chicken breast meat after administration, and the elimination time was 124h. Ceftiofuroxime in chicken kidney was rapidly metabolized as defurfuryl cefotioxime within 0.5 h, and the elimination time of defuryl cefotiofuroxime in chicken liver and kidney was 48 ~ 72 h and 72 ~ 120 h, respectively. This study can provide theoretical and practical basis for the protection of animal food safety, maximum residue limit of cefotaxime in chicken and the period of withdrawal of cefotaxime.
【作者单位】：陕西师范大学;中国检验检疫科学研究院;北京市理化分析测试中心北京市食品安全分析测试工程技术研究中心;北京出入境检验检疫局检验检疫技术中心;厦门市出入境检验检疫局检验检疫技术中心;
【基金】：国家重大仪器开发专项(2012YQ14000806) 北京市科技计划项目(Z141100002614020)资助
【分类号】：O657.63;TS251.7

【相似文献】