气相色谱质谱联用法测定重楼药材中多种农药残留

Determination of Multiple Pesticide Residues in Paridis Rhizoma by Gas Chromatography-Mass Spectrometry

目的建立测定重楼药材中15种农药残留量的气相色谱质谱联用法。方法色谱柱为Agilent 19091S-431UI柱,HP-624毛细管柱(15.0 m×0.25 mm,0.25μm),载气为氦气,流速1.0 mL/min,不分流进样,进样口温度为280℃,程序升温;溶剂延迟时间为3.75 min,进样量为1μL,离子源温度为280℃,传输线温度为280℃,电离方式为电子轰击离子源(EI),能量为70 eV。结果15种成分质量浓度均在0.05~1.0μg/mL范围内与峰面积线性关系良好;定量限为0.010~0.025 mg/kg;精密度、稳定性试验结果的RSD均小于7%;平均加样回收率为78.73%~95.93%,RSD为4.43%~7.41%(n=9)。结论该法前处理简单、快速,分辨率高,能更好地满足检测需求,可用于重楼药材中农药残留的检测。

Objective To establish a gas chromatography-mass spectrometry(GC-MS)method for determining the residues of 15 pesticides in Paridis Rhizoma.Methods The chromatographic columns were the Agilent 19091S-431UI column and HP-624 capillary column(15.0 m×0.25 mm,0.25μm),the carrier gas was helium,the flow rate was 1.0 mL/min,the splitless injection was adopted,the injection inlet temperature was 280℃,the programmed temperature was adopted;the solvent delay time was 3.75 min,the injection volume was 1μL,the ion source temperature was 280℃,the transmission line temperature was 280℃,the electron impact ion source(EI)was adopted with the energy of 70 eV.Results The linear ranges of fifteen components were in the range of 0.05-1.0μg/mL.The limit of quantification(LOQ)was in the range of 0.010-0.025 mg/kg.The RSDs of precision and stability tests were lower than 7%.The average recovery rate was in the range of 78.73%-95.93%with the RSDs of 4.43%-7.41%(n=9).Conclusion This method is simple,fast,and has high resolution,which can better meet the detection needs and can be used for the detection of pesticide residues in Paridis Rhizoma.