中文摘要：

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—ToF MS／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McI lvaine-Na2EDTA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、金霉素的标准曲线砰均大于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·k^-1DW，金霉素浓度范围0．0-19．22mg·kg^-1DW．

英文摘要：

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.