QuEChERS法与UPLC-MS/MS法对土壤中五种磺酰脲类除草剂的快速检测  

Using Qu ECh ERS Method and Ultra-high-pressure Liquid Chromatography Tandem Mass Spectrometry to Rapidly Determine Five Sulfonylurea Herbicides in Soil Samples

作　　者：彭西甜[1] 夏虹[1] 胡西洲[1] 彭立军[1] 祁志红[1] 沈菁[1] 

机构地区：[1]湖北省农业科学院农业质量标准与检测技术研究所,武汉430064

出　　处：《湖北农业科学》2014年第23期5843-5847,共5页Hubei Agricultural Sciences

基　　金：湖北省农业科学院青年基金项目(2013NKYJJ18;2014NKYJJ20)

摘　　要：建立了一种土壤中5种磺酰脲类除草剂高效、快速、灵敏的检测方法。土壤中的磺酰脲残留物似因嘧磺隆、甲磺隆、绿磺隆、胺苯磺隆和苄嘧磺隆）采用缓冲盐改进的OuEChERS法提取．乙腈提取液经浓缩、甲醇／水（1／1，V/V）混合溶剂定容后进入超高效液相色谱一串联质谱（UPLC-MS／MS）进行分析。在优化好的色谱和质谱条件下，对基质效应进行了考察，结果表明。所有分析物体现了明显的基质减弱效应．采用基质匹配的校准曲线进行定量分析。在0．2～100．0μg／kg内，5种磺酰脲除草剂线性方程的R^2大于0．9969，定量限为0．07—0．10μg／kg。在低、中、高3种添加浓度的回收率为75．9％-94．0％，日内日间相对标准偏差小于11．5％．表明所建立的方法在土壤中磺酰脲除草剂的检测上具有潜在的应用前景．A efficient, rapid and sensitive method of determing 5 sulfonylurea herbicides （nicosulfuron, methsulfuron-methyl, chlorsulfuron, ethametsulfuron-methyl and bensulfuron-methyl） in soil was established. The buffered modified QuEChERS （quick, easy, cheap, effective, rugged and safe） method was used to extract the residues of sulfonylurea herbicides. The extracts were concentrated and redissolved with MeOH/H2O （1/1, V/V） to be directly analyzed with ultra-high-pressure liquid chromatography and tandem mass spectrometry （UPLC-MS/MS）. Under the optimized LC and MS conditions, the matrix effects （ME） was investigated and obvious signal suppression was observed for all analytes. Matrix-matched calibrations were used to analyze the residues of sulfonylurea herbicides in soil. Results showed that good linearities in the range of 0.2- 100.0 μg/kg were obtained for all sulfonylurea herbicides with R2 larger than 0.996 9. The limits of quantitation （LOQs） were found to be in the range of 0.07-0.10 μg/kg. The method recoveries of the sulfonylurea herbicides spiked at low, middle and high concentrations in soil samples were from 75.9% to 94.0%, with intra-day and inter-day relative standard deviations less than 11.5%, indicating that the established method has great potential for determing sulfonylurea herbicides in soil samples.

关 键 词：超高效液相色谱-串联质谱(UPLC—MS/MS)法 磺酰脲除草剂 多残留 QuEChERS法 土壤 

分 类 号：O657.72[理学—分析化学]