CAJ | 학술논문

采用超高效液相色谱-串联质谱联用(UPLC-MS/MS)技术建立了同时检测蔬菜中7种氨基甲酸酯类农药多残留量的快速检测方法.样品经乙腈提取,氨基固相萃取柱净化,Waters C_(18)超高效液相色谱柱分离,进入电喷雾串联四极杆质谱进行检测,采用多反应监测(MRM)分析,对液质分离条件和样品前处理条件进行了优化.结果表明7种氨基甲酸酯类农药在2～500 μg/L范围内线性良好(r≥0.9986).在0.005～0.01 mg/kg范围内,平均加标回收率在72.4%～112.1%之间;相对标准偏差小于13%.该方法检出限范围为1.31～3.72 μg/L,测定结果满足多残留农残的检测要求.
채용초고효액상색보-천련질보련용(UPLC-MS/MS)기술건립료동시검측소채중7충안기갑산지류농약다잔류량적쾌속검측방법.양품경을정제취,안기고상췌취주정화,Waters C_(18)초고효액상색보주분리,진입전분무천련사겁간질보진행검측,채용다반응감측(MRM)분석,대액질분리조건화양품전처리조건진행료우화.결과표명7충안기갑산지류농약재2～500 μg/L범위내선성량호(r≥0.9986).재0.005～0.01 mg/kg범위내,평균가표회수솔재72.4%～112.1%지간;상대표준편차소우13%.해방법검출한범위위1.31～3.72 μg/L,측정결과만족다잔류농잔적검측요구.
An ultra performance liquid chromatography-tandem mass spectrometric method (UPLC-MS/MS) has been developed for the simultaneous determination of seven carbamate pesticide residues and the metabolites in vegetables. The carbamate pesticides were extracted with acetonitrile, cleaned up with NH2 solid phase extraction cartridge (SPE). The UPLC analyses were performed on an acquity UPLC C_(18) column with gradient eluation, combined with electrospray ionization in positive mode (ESI+) and multiple reaction monitoring (MRM) mode. The linear range was 2～500 μg/L, and the correlation coefficients were 0.9986～0.9996. The average recoveries of seven carbamate pesticides in spiked vegetables (0.005 and 0.10 mg/kg) ranged from 72.4% to 112.1% and the relative standard deviations were between 0.3% and 12.3%. The results indicate that the method developed is easy, fast, sensitive and has a good purification effect. The multi-residue analysis method can meet the requirements for simultaneous determination of multi-pesticides residues in vegetables.