超高效液相色谱-串联质谱法测定硝磺草酮在稻田中的残留

Determination of mesotrione residues in rice ecosystem by UPLC-MS/MS

建立了利用超高效液相色谱-串联质谱法测定硝磺草酮在糙米、谷壳、植株、土壤和稻田水中残留的方法。样品经乙腈和水(或乙酸乙酯)提取,HLB固相萃取小柱净化,超高效液相色谱-串联质谱检测。结果表明,硝磺草酮在0.005~0.2 mg/L范围内线性关系良好,相关系数为0.9996,硝磺草酮在糙米、谷壳、植株、土壤和稻田水中的回收率为85%~105%,相对标准偏差为3.1%~13.3%。硝磺草酮在糙米中的定量限为0.01 mg/kg,在谷壳和植株中的定量限为0.02 mg/kg,在土壤中的定量限为0.005 mg/kg,在稻田水中的定量限为0.001 mg/L。该方法简便、快速、准确、灵敏度高,可用于稻田中硝磺草酮的残留检测。

A method for determination of mesotrione residues in the husked rice,rice hulls,rice plant,soil and paddy water was developed based on ultrahigh performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).The samples were extracted with acetonitrile and water,purified with an HLB solid phase extraction column,and determined by UPLC-MS/MS.The results showed that the calibration curve for mesotrione was linear in the range of 0.005~0.2 mg/L with correlation coefficients of 0.9996.At different spiked levels,the average recoveries of mesotrione in husked rice,rice hulls,rice plant,soil and paddy water were 85%-105%,and the relative standard deviation(RSD)ranged from 3.1%to 13.3%.The limit of quantitation(LOQ)of mesotrione in husked rice was 0.01 mg/kg,in rice hulls and rice plant were 0.02 mg/kg,in soil was 0.005 mg/kg,in paddy water was 0.001 mg/L.The method is simple,rapid,accurate,and sensitive,and can be adapted for the determination of mesotrione residues in rice paddy.