QuEChERS-GC-MS/MS测定蚓激酶原料药中41种农药残留量

Determination of 41 Pesticide Residues in Lumbrokinase by Modified Qu ECh ERS Method and GC-MS/MS

目的:建立Qu ECh ERS(quick,easy,cheap,effective,rugged and safe)快速样品前处理技术结合气相色谱串联质谱法(GC-MS/MS)同时测定蚓激酶原料药中41种农药残留的方法。方法:采用GC-MS/MS法测定蚓激酶原料药中41种农药残留量。色谱柱为HP-5ms ultla Lert弹性石英毛细管柱(30.0 m×0.25 mm,0.25μm),检测器为质谱检测器,进样口温度为240℃;检测器温度为280℃,程序升温,载气为高纯氦气,隔垫吹扫为5 ml·min^-1,柱流速为2.0 ml·min^-1,进样量为1.0μl,进样方式为不分流。质谱检测器离子源为电子轰击离子源,离子源温度为230℃,碰撞气为高纯氩气,灯丝电压为70 e V,传输线温度为280℃,积分延时为4 min。结果:41种农药检测质量浓度线性范围均为100~500μg·L^-1(r≥0.995 0);检测限为1.5~3.8μg·L^-1;定量限为5.0~12.5μg·L^-1;精密度的RSD均<8%(n=6)、重复性与稳定性试验的RSD均<6%(n=6);蚓激酶原料药样品加样平均回收率均为70.47%~105.66%。结论:该方法简便、准确、高效,可用于判断蚓激酶原料药是否有农药残留。

Objective: To apply a modified quick,easy,cheap,effective,rugged and safe( Qu ECh ERS) approach in the determination of 41 pesticides in lumbrokinase by GC-MS/MS. Methods: GC-MS/MS was used to determine 41 pesticide residues in lumbrokinase. The column was an HP-5 ms ultla Lert fused silica capillary column( 30. 0 m × 0. 25 mm,0. 25 μm),the detector was the mass spectrometer detector,the inlet temperature was 240℃,the detector temperature was 280℃ with programming,and the carrier gas was helium with high purity. The spacer purging was 5 ml·min^-1,the column flow rate was 2. 0 ml·min^-1,and the injection volume was 1. 0 μl. The injection mode was without shunt. The ion source of the mass spectrometer detector was an electron bombardment ion source with the temperature at 230 ℃. The collision gas was argon with high purity. The filament voltage was 70 e V,the transmission line temperature was 280 ℃,and the integration delay was 4 min. Results: The linear range of the 41 pesticides was 100-500 μg·L-1( r≥0. 995 0). The detection limit was 1. 5-3. 8 μg·L^-1. The quantitative limit was 5. 0-12. 5 μg·L^-1. The RSD of precision was less than 8%( n = 6),and that of repeatability and stability test was less than 6%( n = 6). The recoveries were within the range of70. 47%-105. 66%. Conclusion: The method is simple,accurate and efficient,and can be used to determine whether lumbrokinase contains pesticide residues.