畜禽养殖活体动物体液中多种激素类药物残留监测方法研究  

Study on Monitoring Methods for Multihormone Drug Residues in Livestock and Poultry Livestock Fluid

作　　者：张彤 刘瑜 李晓东 付海滨 刘俊 林华 薛志平[1] 张敏[1] ZHANG Tong;LIU Yu;LI Xiaodong;FU Haibin;LIU Jun;LIN Hua;XUE Zhiping;ZHANG Min(College of Engineering,Shenyang Agricultural University,Shenyang 110866;Technology Center of Shenyang Customs,Shenyang 110016;Technology Center of Chengdu Customs,Chengdu 610041)

机构地区：[1]沈阳农业大学工程学院,辽宁沈阳110866 [2]沈阳海关技术中心,辽宁沈阳110016 [3]成都海关技术中心,四川成都610041

出　　处：《分析科学学报》2023年第6期672-678,共7页Journal of Analytical Science

基　　金：国家重点研发计划(2022YFF1100804);辽宁省自然科学基金项目(20170520089);四川省科技计划项目(2023JDRC0007);辽宁省自然科学基金项目(2022HK021);沈阳市科技计划项目(21-108-9-37)。

摘　　要：本研究通过优化样品前处理和仪器检测条件,采用QuEChERS前处理技术结合超高效液相色谱-串联质谱法建立了动物体液中雌激素、孕激素、雄激素、糖皮质激素等17种激素同时测定的分析方法。试样以β-葡萄糖醛酸酶/芳香基硫酸酯酶进行酶解,经乙腈提取,QuEChERS净化,采用C18色谱柱分离,流动相为乙腈+水,质谱扫描模式为多反应监测(MRM),内标法定量。结果显示,方法的检出限为0.15~0.30μg/L,定量限为0.5~1.0μg/L,回收率为72.8%~107.1%,相对标准偏差为0.9%~9.6%。该方法简便、快速、准确,适用于动物体液中17种激素的同时检测。An analytical method was established for the simultaneous determination of 17 hormones in animal body fluids,including estrogen,progesterone,androgen,and glucocorticoids,using QuEChERS combined with ultra-high performance liquid chromatography-tandem mass spectrometry.Sample was enzymatically hydrolyzed withβ-Glucuronidase/arylsulfatase,extracted with acetonitrile,purified with QuEChERS,and separated using a C18 chromatographic column with acetonitrile and water as the mobile phase.The mass spectrometry scanning mode was multi reaction monitoring(MRM),and the internal standard method was used for quantification.The detection limit of this method is 0.15-0.30μg/L,with a quantification limit of 0.5-1.0μg/L,recovery of 72.8%-107.1%,relative standard deviation of 0.9%-9.6%.This method is simple,fast,and accurate,and is suitable for the simultaneous detection of 17 hormones in animal body fluids.

关 键 词：激素 液相色谱-串联质谱 动物体液 QUECHERS 

分 类 号：O657.63[理学—分析化学]