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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.
In this study, UPLC / Q-ToFMS / MS was established for the determination of residual oxytetracycline, EDTA buffer and ultrasonic extraction, SPE solid-phase extraction, using ultra-performance liquid chromatography, ultraviolet detection of external standard quantitative, quadrupole-time of flight tandem mass spectrometry positive mode.When 0.5mg · kg-1DW- The standard curves of oxytetracycline, tetracycline and chlortetracycline were both greater than 0.99 and the relative standard deviation was less than 3%. The average recoveries of spiked samples were between 70.0% and 113.0% in the range of 10mg · kg-1DW (dryweight) Using this method, the detection of oxytetracycline, tetracycline and chlortetracycline can be completed in 5min, their detection limits were 0.1mg · kg-1, 0.1mg · kg-1 and 0.2mg · kg-1, respectively. The detection results of swine manure samples from 10,000 pig farms in the region showed that all the three tetracyclines were detected in varying degrees, with oxytetracycline concentration ranging from 10.5 mg · kg-1DW-513.4 mg · kg-1DW and tetracycline concentration ranging from 12.53 -77.10 mg · kg-1DW, chlortetracycline concentration range 0.0-19.22 mg · kg-1DW.