液质联用技术检测紫薯蓣中5种氨基甲酸酯农药的方法研究
Simultaneous determination of carbamate pesticide residues in purple yam by high performance liquid chromatography-tandem mass spectrometry
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摘要: 通过超高液相色谱-串联质谱联用(LC-MS/MS)技术,建立了一种高灵敏度检测紫薯蓣中农药残留的方法。样品经环己烷-乙酸乙酯(1∶1,V/V)提取,全自动凝胶净化在线浓缩仪净化,然后采用LC-ESI(+)-MS/MS测定,对液质分离条件进行优化。实验结果表明,5种氨基甲酸酯农药在1.050.0μg/L范围内线性关系良好,相关系数0.99830.9999;在2.010.0μg/kg浓度范围内,加样回收率82.05%97.27%之间,相对标准偏差2.85%6.63%。该方法具有快速、准确、简便、灵敏、净化效果好、人为误差小的特点。Abstract: The high sensitive liquid chromatography-tandem mass spectrometry ( LC-MS/MS) had been developed for the detection of 5 carbamate pesticides in purple yam.After extraction of the pesticides with cyclohexane and ethyl acetate ( v /v = 1∶1) , the extract was purified by automatic gel purification system using cyclohexane and ethyl acetate ( v /v = 1 ∶ 1) as mobile phase.Analysis was performed by liquid chromatography- electrospray ionization-tandem mass spectrometry operated in the multiple reaction monitoring ( MRM) mode, and the separation conditions were optimized.The results showed that calibration curves were linear and covered from 1.0 to 50.0μg /L, and the correlation coefficients was 0.99830.9999.The average recoveries, measured at 2.0 to 10.0μg /kg, were in the range82.05% to 97.27% for all of the compounds tested with relative standard deviations were between 2.85% to 6.63%.The results indicated that the method had been demonstrated to be simple, accurate, practical and high sensitive for the determination of carbamates residues in purple yam samples.