为快速检测大豆中硝磺草酮残留量建立了高效液相色谱–串联质谱的新方法。大豆样品采用乙腈提取,Na Cl盐析,十八(烷)基硅烷(C_(18))和石墨化炭黑(GCB)分散固相萃取净化,以phenomenex Luna 3u C_(18)(2)100A柱为分离柱,用乙腈和0.1%氨水溶液进行梯度洗脱,电喷雾负离子(ESI^–)多反应监测,高效液相色谱–串联质谱(HPLC–MS/MS)测定。本方法条件下,硝磺草酮在0.0075–0.75μg/m L浓度范围内呈良好的线性关系(R^2〉0.997),方法检出限(LOD)和定量限(LOQ)分别为0.0009和0.003 mg/kg。在0.003、0.03和0.3 mg/kg添加水平下,硝磺草酮的日内平均回收率为83.84–96.24%,日内相对标准偏差(RSD)为1.99–3.78%,日间平均回收率为85.13–95.25%,日间RSD为2.11–3.47%,能满足大豆中硝磺草酮检测的要求。
A novel Qu ECh ERS method was developed for the rapid determination of mesotrione residue in soybean using high performance liquid chromatography tandem-mass spectrometry( HPLC – MS/MS). The samples were extracted with acetonitrile,then salted out with Na Cl,purified with GCB and Cl8,separated on a phenomenex Luna 3u C_(18)( 2) 100 A column with gradient elution by using acetonitrile and 0.1% ammonia aqueous as eluant,and detected by HPLC – MS/MS under negative electrospray ionization( ESI~–) and multiple-reaction monitoring( MRM) models. Under these conditions,mesotrione showed a good linear relationship( R2〉0.997) in the concentration range of 0.0075 – 0.75 μg/m L,and the limit of quantification( LOQ) and limit of detection( LOD) in soybean were 0.003 and 0.0009 mg/kg,respectively. Three spiked levels at 0.003,0.03 and 0.3 mg/kg were investigated,and the intra-day average recoveries ranged from 83.84% to 96.24%,with intra-day relative standard deviations( RSDs) of 1.99 "3.78%,the inter-day average recoveries ranged from 85.13% to 95.25%,inter-day RSDs of 2.11 " 3.47%,which met the requirement of mesotrione determination in soybean.