Suppr超能文献

超高效液相色谱-串联质谱法同时测定鸡肝中四环素类、磺胺类和喹诺酮类药物残留

[Simultaneous determination of tetracyclines, sulfonamides and quinolones residues in chicken livers by ultra performance liquid chromatography-tandem mass spectrometry].

作者信息

Guo Liming, Zhu Kui, Jiang Haiyang, Li Jiancheng, Li Xiaowei, Ding Shuangyang

机构信息

College of Veterinary Medicine, China Agricultural University, Beijing, China.

出版信息

Se Pu. 2009 Jul;27(4):412-6.

Abstract

An analytical method for the simultaneous determination of 3 tetracyclines, 10 sulfonamides and 8 quinolones in chicken livers by ultra performance liquid chromatography coupled with tandem quadrupole mass spectrometry (UPLC-MS/MS) in positive ion mode with multiple reaction monitoring (MRM) has been developed and validated. A total of 2 g homogenized sample of chicken livers was placed in a 50 mL polypropylene tube, and 1 mL of McIlvaine buffer and 4 mL of acetonitrile were added. After stirring and centrifuging for 5 min at 4,000 r/min, the supernatant was collected and the remains was extracted by 5 mL acetonitrile. The supernatant was merged together and evaporated to dryness under a steam of nitrogen at 60 degrees C. The residue was dissolved with 4 mL of phosphoric acid-triethylamine buffer-acetonitrile (85:15, v/v) and 4 mL of n-hexane. After stirring for 1 min and centrifuging for 5 min at 4 000 r/min, the under layer solution was analyzed using UPLC-MS/MS. The satisfactory recoveries (66.8% - 128.5%) of all the veterinary drugs were demonstrated at spiked levels of 5, 10 and 50 microg/kg with the overall relative standard deviations (RSDs) for intra-day and inter-day of the 21 analytes less than 20.5%. The limit of detection (LOD) and the limit of quantification (LOQ) were 2 microg/kg and 5 microg/kg, respectively for each drug. This method has good stability, lower detection limits and can be used as a conclusive evidence method of these drug residues in chicken livers.

摘要

建立并验证了一种超高效液相色谱-串联四极杆质谱法(UPLC-MS/MS),以正离子模式和多反应监测(MRM)同时测定鸡肝中3种四环素类、10种磺胺类和8种喹诺酮类药物。取2g鸡肝匀浆样品置于50mL聚丙烯管中,加入1mL麦氏缓冲液和4mL乙腈。搅拌并于4000r/min离心5min后,收集上清液,剩余物用5mL乙腈萃取。将上清液合并,在60℃氮气气流下蒸发至干。残渣用4mL磷酸-三乙胺缓冲液-乙腈(85:15,v/v)和4mL正己烷溶解。搅拌1min并于4000r/min离心5min后,取下层溶液用UPLC-MS/MS分析。在5、10和50μg/kg的加标水平下,所有兽药的回收率均令人满意(66.8%-128.5%),21种分析物的日内和日间总体相对标准偏差(RSD)均小于20.5%。每种药物的检测限(LOD)和定量限(LOQ)分别为2μg/kg和5μg/kg。该方法稳定性好,检测限低,可作为鸡肝中这些药物残留的确证方法。

文献检索

告别复杂PubMed语法,用中文像聊天一样搜索,搜遍4000万医学文献。AI智能推荐,让科研检索更轻松。

立即免费搜索

文件翻译

保留排版,准确专业,支持PDF/Word/PPT等文件格式,支持 12+语言互译。

免费翻译文档

深度研究

AI帮你快速写综述,25分钟生成高质量综述,智能提取关键信息,辅助科研写作。

立即免费体验