气相色谱-三重四级杆质谱法测定土壤中丙炔氟草胺

Determination of Flumioxazin in Soil by Gas Chromatography-Triple Quadrupole Mass Spectrometry

建立气相色谱-三重四级杆质谱法测定土壤中丙炔氟草胺的方法。样品经过乙腈提取,无水硫酸镁除水、C18净化,以空白基质匹配标准曲线外标法、选择离子监测(SRM)定性、定量。在0.02~1.0mg/kg内丙炔氟草胺具有较好的线性关系(相关系数≥0.995),方法定量限(LOQ)为0.02mg/kg。在空白基质加标0.02、0.1、0.5mg/kg的水平下,其回收率为85.4%~108.8%,精密度(相对标准偏差,RSD)<15%。该方法选择性较好,其定量限、回收率及精密度可以满足实际土壤样品中丙炔氟草胺的检测。

A Gas Ghromatography-Triple Quadrupole Mass Spectrometry method was established for the determination of Flumioxazin residue in soil. The samples were extracted with acetonitrile, dewatered by magnesium sulfate, and purified by C18. Flumioxazin was identified with selected ion monitoring(SRM) and quantified with blank matrix-matched external standard method. In the range of 0.02~1.0mg/kg, the method showed a good linearity(correlation coefficient ≥ 0.995),and the limit of quantification(LOQ) is 0.02mg/kg. When the blank matrix is spiked with 0.02mg/kg, 0.1mg/kg, 0.5mg/kg, the recoveries of flumioxazin were between 85.4% to 108.8%,with the precision(relative standard deviation, RSD) of less than 15%. All the method parameters including selectivity, limit of quantification, recovery and precision meet the criteria for the detection of Flumioxazin residue in actual soil samples.