CAJ | 학술논문

建立了超高效液相色谱?四极杆?飞行时间质谱（ UPLC?Q?TOF MS）快速检测猪肉中6类33种兽药残留的分析方法。样品采用QuEChERS方法进行前处理（5％（v／v）乙酸乙腈溶液提取，C18和 NH2吸附剂净化），采用ZORBAX SB?C18色谱柱（100 mm×2?1 mm，3?5μm）分离，以乙腈?0?1％（v／v）甲酸水溶液（含5 mmol／L乙酸铵）为流动相，梯度洗脱，Q?TOF MS电喷雾正离子模式分析检测。在全扫描采集模式下，以准分子离子峰的峰面积定量，以化合物的色谱保留时间和精确质量数定性。在Target MS／MS采集模式下，通过碎片离子的精确质量数进一步确证化合物。33种化合物在各自的线性范围内均呈现良好的线性关系，相关系数均大于0?99，33种化合物的定量限（S／N＝10）为2?5～100μg／kg，添加回收率为67?0％～109?0％，相对标准偏差（RSD， n＝6）均不高于15?1％。该方法简便、快速、灵敏，适用于猪肉中多类兽药残留的同时检测。
건립료초고효액상색보?사겁간?비행시간질보（ UPLC?Q?TOF MS）쾌속검측저육중6류33충수약잔류적분석방법。양품채용QuEChERS방법진행전처리（5％（v／v）을산을정용액제취，C18화 NH2흡부제정화），채용ZORBAX SB?C18색보주（100 mm×2?1 mm，3?5μm）분리，이을정?0?1％（v／v）갑산수용액（함5 mmol／L을산안）위류동상，제도세탈，Q?TOF MS전분무정리자모식분석검측。재전소묘채집모식하，이준분자리자봉적봉면적정량，이화합물적색보보류시간화정학질량수정성。재Target MS／MS채집모식하，통과쇄편리자적정학질량수진일보학증화합물。33충화합물재각자적선성범위내균정현량호적선성관계，상관계수균대우0?99，33충화합물적정량한（S／N＝10）위2?5～100μg／kg，첨가회수솔위67?0％～109?0％，상대표준편차（RSD， n＝6）균불고우15?1％。해방법간편、쾌속、령민，괄용우저육중다류수약잔류적동시검측。
An analytical method was established for the simultaneous determination of six clas?ses of 33 veterinary drug residues in pork by ultra performance liquid chromatography coupled with quadrupole?time of flight mass spectrometry ( UPLC?Q?TOF MS ) . The QuEChERS method has been validated for the extraction. In this method, the sample was extracted by acetonitrile containing 5%( v/v) acetic acid and cleaned?up with C18 and NH2 adsorbents. The extract was measured directly by UPLC?Q?TOF MS with electrospray ionization in positive mode. The com?pounds were separated on a ZORBAX SB?C18 column (100 mm×2?1 mm, 3?5μm) with acetoni?trile?0?1% formic acid containing 5 mmol/L ammonium acetate as mobile phases under gradient elution. The confirmatory analysis was carried out by determining the retention times and accu?rate masses of all the compounds and fragment ions upon Target MS/MS. The correlation coeffi?cients of the 33 veterinary drugs were more than 0?99 within their linear ranges. The limits of quantification ( LOQs) were 2?5-100 μg/kg. The recoveries ranged from 67?0% to 109?0% with the relative standard deviations ( RSDs, n=6) not more than 15?1%. The method is rapid, sensi?tive, and suitable for the simultaneous determination of multi?classes of veterinary drugs in pork.