超高效液相色谱串联质谱检测猪粪中残留的四环素类抗生素  

DETERMINATION OF TETRACYCLINES RESIDUES IN SWINE MANURE BY UPLC/MS

作　　者：沈颖[1] 魏源送[1] 郭睿[1] 徐超一[2] 张朝晖[2] 周光漪[2] 赵鑫[2] 刘俊新[1] 

机构地区：[1]中国科学院生态环境研究中心,北京100085 [2]北京出入境检验检疫局,北京100026

出　　处：《环境化学》2009年第5期747-752,共6页Environmental Chemistry

基　　金：国家863计划项目(No.2007AA06Z344);国家自然科学基金项目(No.50578156)

摘　　要：本研究建立了超高效液相色谱/四极杆-飞行时间串联质谱(UPLC/Q-ToFMS/MS)测定猪粪中残留土霉素、四环素和金霉素的方法.样品分别经McⅠlvaine-Na2 EDTA缓冲液和超声提取、SPE固相萃取后,采用超高效液相色谱分离,紫外检测外标法定量,四级杆-飞行时间串联质谱仪正离子模式定性.在0.5mg·kg-1DW—10mg·kg-1DW(dryweight)范围内,土霉素、四环素、金霉素的标准曲线R2均大于0.99,相对标准偏差小于3%,样品加标平均回收率在70.0%—113.0%之间;采用该方法,土霉素、四环素和金霉素的检测可在5min内完成,它们的检出限分别为0.1mg·kg-1,0.1mg·kg-1和0.2mg·kg-1.北京地区万头养猪场猪粪样品的检测结果表明,这3种四环素均有不同程度的检出,其中土霉素浓度范围10.5mg·kg-1DW—513.4mg·kg-1DW,四环素浓度范围12.53—77.10mg·kg-1DW,金霉素浓度范围0.0—19.22mg·kg-1DW.A method was developed in this study for analysis of residual tetracycline （TC）, chlortetracycline （CTC） and oxytetracycline （OTC） in swine manure. This method used Mc I lvaine-Na2 EDTA buffer as extraction solution and solid-phase extraction （SPE）followed by an ultra performance liquid chromatography/hybrid quadrupole time of flight mass spectrometer （UPLC/Q-ToF MS/MS） with positive ion electrospray. At the spiked concentrations ranging from 0. 5--10.0 mg· kg^-1 DW （ dry weight）, all the coefficients （R^2 ） of standard curves of OTC, TC and CTC were more than 0. 99, and their relative standard deviations were less than 3%. The quantitative recoveries of OTC, TC and CTC were in the range of 70. 0% and 113.0%. The analysis of OTC, TC and CTC could be done within 5 minutes by the UPLC/Q-ToF MSMS, and the method detection limits（ MDL） were 0.1mg·kg^-1 DW, 0.1mg· kg^-1 DW and 0. 2mg·kg^-1 DW for OTC, TC and CTC, respectively. Investigation results of concentrated swine farms in Beijing showed that all these three tetracyclines were detected in swine manure, including 10. 5-513.4 mg·kg^-1 DW of OTC, 12. 53--77. 10 mg· kg^-1 DW of TC, and 0.0-19.22 mg· kg^-1 DW of CTC.

关 键 词：四环素类抗生素 残留量 检测 猪粪 超高效液相色谱. 

分 类 号：S859.8[农业科学—临床兽医学]