CAJ | 학술논문

利用液相色谱-四极杆-飞行时间质谱技术，对7类45种兽药残留同时检测方法进行探究。经BAP-SPE固相萃取柱富集净化，甲醇、1%甲酸乙腈和10%甲醇乙酸乙酯依次洗脱，吹干后纯水-乙腈（V/V，9∶1）定容上机检测。45种目标物经Agilent Extend C18型色谱柱分离，分别以含0.1%甲酸的5 mM乙酸铵-乙腈为流动相进行ESI+正离子采集和5 mM乙酸铵-乙腈为流动相进行ESI-负离子采集。结果显示，7类45种兽药在1~500μg/L时线性关系良好，相关系数均大于0.99，仪器测定低限LOD在0.50~20.00μg/L，方法检出限均在0.25μg/L以下。除磺胺胍回收率为58.85%外，其余目标物回收率均在70.22%~120.69%，相对标准偏差RSD为1.18%~22.03%。该方法灵敏度高、准确性好，满足兽药多残留的筛查检测要求。
이용액상색보-사겁간-비행시간질보기술，대7류45충수약잔류동시검측방법진행탐구。경BAP-SPE고상췌취주부집정화，갑순、1%갑산을정화10%갑순을산을지의차세탈，취간후순수-을정（V/V，9∶1）정용상궤검측。45충목표물경Agilent Extend C18형색보주분리，분별이함0.1%갑산적5 mM을산안-을정위류동상진행ESI+정리자채집화5 mM을산안-을정위류동상진행ESI-부리자채집。결과현시，7류45충수약재1~500μg/L시선성관계량호，상관계수균대우0.99，의기측정저한LOD재0.50~20.00μg/L，방법검출한균재0.25μg/L이하。제광알고회수솔위58.85%외，기여목표물회수솔균재70.22%~120.69%，상대표준편차RSD위1.18%~22.03%。해방법령민도고、준학성호，만족수약다잔류적사사검측요구。
This paper aim at exploring a method for 7 kinds of 45 veterinary drug residues detection by using liquid chromatography-quadrupole-time-of-flight (LC-Q-TOF) tandem mass spectrometry. By using BAP-SPE solid phase to extract and purity, MeOH, Acetonitrile containing 1.0%(V/V) formic acid and Ethyl Acetate containing 10%(V/V) MeOH to elute successively, vaporat by a streamof nitrogen then add purity water-ACN (V/V, 9∶1) to be ready for injection. The 45 target compounds are separated by Agilent Extend C18 column with the gradient elution using two mobile phases and two different acquisition modes seperately: acetonitrile and 5 mM ammonium acetate mobile phase containing 0.1% formic acid with ESI+ mode, and acetonitrile and 5 mM ammonium acetate mobile phase with ESI- mode. The results show that the 7 kinds of 45 veterinary drugs had good relationshiop in range of 1~500μg/L, the linear correlation coefficient are greater than 0.99, LOD of instrument is 0.50~20.00μg/L, LOD of method is lower than 0.25μg/L. Despite SGD recovery rate is 58.85%, all rest recovery rates are 70.22%~120.69%, the relative standard deviation are 1.18%~22.03%. This method has high sensitivity and good accuracy, which can be used to screen the multi-veterinary residues.