高效液相色谱-串联质谱法测定牛干巴中敌百虫的方法研究

Determination of trichlorfon in nigganba by high performance liquid chromatography-tandem mass spectrometry

研究了前处理方法对高效液相色谱-串联三重四级杆质谱法测定牛干巴中敌百虫残留量的影响。样品使用正己烷去除油脂,再经乙腈萃取浓缩,以乙腈-含0.1%甲酸的10 mmol/L甲酸铵水溶液为流动相,用Agilent C18色谱柱进行梯度洗脱分离,采用ESI正模式电离,多级反应监测(MRM)模式进行检测,外标法定量。结果显示,牛干巴中敌百虫残留量的检出限和定量限分别为0.5μg/kg和1.8μg/kg,在5 ng/mL^100 ng/mL浓度范围内,线性关系良好(R2=0.99936),1μg/kg、2μg/kg、10μg/kg3个加标浓度的回收率均在91.22~100.34,相对标准偏差均小于10%。

Effects of pretreatment on the determination of residual insecticides in bovine dried rice by high performance liquid chromatography-tandem triple quadrupole mass spectrometry were studied.The samples were removed with n-hexane,then extracted and concentrated with acetonitrile.Acetonitrile-10 mmol/L ammonium formate solution containing 0.1%formic acid was used as mobile phase.The samples were separated by gradient elution using Agilent C18 chromatographic column.The results showed that the detection limit and quantitative limit of residual insecticidal residues in nigganba were 0.5μg/kg and 1.8μg/kg respectively,and the linear relationship was good(R2=0.99936)within the concentration range of 5 ng/mL^100 ng/mL.The recoveries of the 3 labeled concentrations of 1μg/kg、2μg/kg and 10μg/kg were all 91.22~100.34,and the relative standard deviation was less than 10%.