【摘要】 建立了SPE/RRLC-MS法定量测定水中除草剂苯噻草胺残留量的方法。固相萃取小柱为SupelcleanTMENVITM-18柱(3 mL);采用快速高分离液相色谱系统进行色谱分离;质谱在正离子扫描模式下,选择丰度最高的碎片离子m/z 192为定量离子,m/z 148为定性参比离子,外标法定量。研究结果显示:方法的仪器检出限(LOD)为0.001 mg/L,理论检出限为0.004μg/L,方法的定量限为0.004 mg/L,线性范围在0.004~0.5 mg/L之间,低、中和高3个浓度点的平均加标回收率为72.1%~97.7%,相对标准偏差(RSD)为3.2%~15%。该方法可用于饮用水和松花江水中苯噻草胺残留量的检测。更多还原

【Abstract】 A SPE-RRLC-MS method was developed for the determination of herbicide mefenacet residue in water samples quantificationally.The SPE pillaret was supelcleanTM ENVITM-18(3 mL);the rapid resolution LC system was applied chromatographic separation;Mass spectrometry was operated under the positive ion mode.The most abundant fragment ion m/z 192 was confirmed to be the quantitative ion for quantification measured by MRM mode with external standard method,m/z 148 was selected to be the qualitative reference ion.The researching results showed that the good linearity was obtained in the range of 0.004～0.5 mg/L with the correlation coefficient(r) of 0.9991.The instrumental detection limit was 0.001 mg/L and the detection limit for theoretical method was 0.004 μg/L;the limit of quantification was 0.004 mg/L;the mean recoveries were between 72.1% and 97.7% at three spiked levels of 0.004,0.05 and 0.5 mg/L with the relative standard deviations of 3.2%～15%.The proposed method was applied to the determination of mefenacet residue in drinking water and songhuajiang river.更多还原