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超高效液相色谱-串联质谱法测定猪组织中泰拉霉素及其代谢物残留量
引用本文:李 建,魏紫嫣,王佳雅,张晶晶,黄川邻,王利丹,孙志文,叶能胜.超高效液相色谱-串联质谱法测定猪组织中泰拉霉素及其代谢物残留量[J].中国兽药杂志,2020,54(5):30-40.
作者姓名:李 建  魏紫嫣  王佳雅  张晶晶  黄川邻  王利丹  孙志文  叶能胜
作者单位:国家粮食和物资储备局科学研究院,,,,,,,首都师范大学化学系
基金项目:北京市科学技术委员会北京市科技重大专项( D171100002017004)
摘    要:对猪组织中泰拉霉素及其代谢物残留量的测定方法进行了研究,基于超高效液相色谱-串联质谱建立了猪肉、肝脏、肾脏中泰拉霉素及其代谢物残留量的测定方法。试样经乙腈-0.1%甲酸水(7+3)提取,MCX柱净化,氮吹后用乙腈-0.1%甲酸水(1+9)复溶,正离子扫描,多反应监测模式下上机分析,基质外标法定量。结果表明,泰拉霉素及其代谢物在5~500μg/kg的浓度范围内呈现良好的线性关系,相关系数(R2)均>0.99;该方法的检出限为5μg/kg(猪肉:2μg/kg),定量限为10μg/kg;在不同浓度添加水平下,平均回收率为72.6%~105.8%,日内相对标准偏差为0.5%~12.1%,日间相对标准偏差为2.9%~8.1%。该方法简便、快速、灵敏度高、重现性好,适用于猪组织中泰拉霉素及其代谢物残留量的测定。

关 键 词:超高效液相色谱-串联质谱法  泰拉霉素  猪组织
收稿时间:2020/1/3 0:00:00
修稿时间:2020/4/18 0:00:00

Determination of Tulathromycin and its Metabolites in pig tissue by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry
LI Jian,WEI Zi-yan,WANG Jia-ya,ZHANG Jing-jing,HUANG Chuan-lin,WANG Li-dan,SUN Zhi-wen,YE Neng-sheng.Determination of Tulathromycin and its Metabolites in pig tissue by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Chinese Journal of Veterinary Drug,2020,54(5):30-40.
Authors:LI Jian  WEI Zi-yan  WANG Jia-ya  ZHANG Jing-jing  HUANG Chuan-lin  WANG Li-dan  SUN Zhi-wen  YE Neng-sheng
Institution:Academy of National Food and Strategic Reserves Administration,,,,,,,
Abstract:A method for the determination of tulathromycin and its metabolite in pig tissues was developed by ultra-high performance liquid chromatography-tandem mass spectrometry.The samples were extracted by acetonitrile-0.1%formic acid aqueous(7+3)and cleaned by MCX solid phase extraction column,and the residue was redissolved with acetonitrile-0.1%formic acid aqueous(1+9)after the dried under a N2 atmosphere.In the positive ion mode and multi reaction monitoring mode,the analytes were quantified by matrix external standard.The results of tulathromycin and its metabolite were linear in the range of 5~500μg/kg with the correlation coefficients(R2)>0.99.The limits of detection(LODs)and the limits of quantification(LOQs)were 5μg/kg(2μg/kg for pork)and 10μg/kg,respectively.The average recoveries of tulathromycin and its metabolite under different spiked levels were 72.6%~105.8%with intraday relative standard deviations(RSDs)of 0.5%~12.1%and interday relative standard deviations(RSDs)of 2.9%~8.1%.The method was easy,fast,highly sensitive and fine reproducibility,and was suitable for the determination of tulathromycin and its metabolite in pig tissues.
Keywords:ultra-high performance liquid chromatography-tandem mass spectrometry  tulathromycin  pig tissues
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