农药学学报2017，Vol.19Issue(1)：53-60,8.DOI:10.16801/j.issn.1008-7303.2017.0008
固相萃取-高效液相色谱-串联质谱法检测稻田中硝磺草酮和2甲4氯钠残留
Determination of mesotrione and MCPA-Na residues in Oryza sativa ecosystems by solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
A rapid multi-residue analytical method for the simultaneous determination of mesotrione and MCPA-Na was developed using dispersive solid phase extraction and high performance liquid chromatography-tandem mass spectrometry(SPE-LC-MS/MS). The analytes were extracted by ethyl acetate, cleaned up by PSA and C18 solid phase extraction column, and separated on a reversed phase C18 column using a gradient elution program with 0.1% aqueous formic acid and 0.1% methanol formic acid as the mobile phase. Quantitative analysis was performed with electrospray ionization in positive/negative mode (ESI+) /(ESI-) under multiple reaction monitoring(MRM) mode. In this study, the LODs of mesotrione and MCPA were 0.005 ng and 0.025 ng, respectively, and LOQ were 0.01 and 0.05 mg/L, respectively. When the addition levels ranging from 0.001 to 2 mg/L mesotrione and from 0.005 to 5 mg/L MCPA, there was a good linear relationship between the mass concentration and the corresponding peak area, and the correlation coefficients were higher than 0.9997. When the addition level ranged from 0.01 to 2 mg/L, the average recovery of mesotrione in water, paddy soil, rice plant, rice husk and brown rice was 75%-103%, and the relative standard deviation (RSD) ranged from 0.1%to 8.2%; when it ranged between 0.05-10 mg/L, the average recovery rate of MCPA in water, paddy soil, rice plant, rice husk and brown rice rate was between 90%-113%, and the RSD was between 0.5%-7.4%. Results indicated that this method is highly efficient, with good sensitivity and accuracy, which can meet the detection requirements of mesotrione and MCPA residues in Oryza sativa ecosystem samples.关键词
固相萃取/高效液相色谱-串联质谱/硝磺草酮/2甲4氯钠/残留/稻田Key words
solid-phase extraction/high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)/mesotrione/MCPA-Na/residue/rice ecosystem分类
农业科技引用本文复制引用
吴晓峰,欧晓明,金晨钟,梁骥,刘秀,李成业,孔玄庆..固相萃取-高效液相色谱-串联质谱法检测稻田中硝磺草酮和2甲4氯钠残留[J].农药学学报,2017,19(1):53-60,8.基金项目
湖南省高校产业化培育项目 (13CY030) （13CY030）
湖南省高校创新平台开放基金项目 (15K066) （15K066）
湖南人文科技学院产学研合作引导项目 (2013CXY04) （2013CXY04）
湖南省2015年研究生创新科研项目 (CX2015B596). （CX2015B596）
