改进的QuEChERS-HPLC-MS/MS法测定噻虫胺在水稻和土壤中的残留  

Clothianidin Residues in Rice and Soil by Modified QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：纪明山[1] 程功[1] 刘娜[1] 谷祖敏[1] 白雪松[1] 姜震[1] 尚涛[1] 杜颖[1] 

机构地区：[1]沈阳农业大学植物保护学院,沈阳110866

出　　处：《农药》2017年第5期361-363,371,共4页Agrochemicals

摘　　要：[目的]建立一种检测水稻和土壤中噻虫胺残留的分析方法。[方法]采用改进的分散固相萃取-高效液相色谱-串联质谱(QuEChERS-HPLC-MS/MS)法,样品经乙腈提取,采用C_(18)、N-丙基乙二胺(PSA)和石墨化炭黑(GCB)作为分散固相萃取(DSPE)的吸附材料,C_(18)色谱柱分离,乙腈-0.2%甲酸水溶液为流动相,梯度洗脱,在电喷雾离子源(ESI)、正离子多反应监测模式(MRM)下测定。[结果]噻虫胺0.01~1 mg/kg添加水平下,平均添加回收率在76.6%~101.0%之间,日内相对标准偏差在1.0%~7.7%之间(n=5),日间相对标准偏差在1.7%~10.2%之间(n=15)。LOD和LOQ分别为0.1~0.2、0.2~0.5μg/kg。[结论]该方法简单、准确,适合于噻虫胺的定性和定量分析。[Aims] The aims were to establish an analytical method for the determination of clothianidin residues in rice and soil. [Methods] The samples were extracted with acetonitrile, C18, PSA and GCB were used as sorbents in the DSPE procedure. The clothianidin residues were analyzed by HPLC-MS/MS, which equipped with an Eclipse Plus C18 column using a gradient elution program and with the mixture of 0.2% formic acid and acetonitrile as the mobile phase. The analysis program was performed with electro-spray ionization in positive mode （ESI＋） under the multipIe reaction monitoring （MRM） mode. [Results] When the addition levels were 0.01-1 mg/kg, the average recovery rates were 76.6- 101.0%, the relative standard deviations were 1.0-7.7% （n=5） and 1.7-10.2% （n=15）. The LOD and LOQ were 0.1-0.2 and 0.2-0.5 μg/kg, respectively. [Conclusions] The method is simple, accurate and suitable for the qualitative and quantitative analysis ofclothianidin.

关 键 词：QUECHERS 高效液相色谱串联质谱法 噻虫胺 水稻 土壤 

分 类 号：O657.63[理学—分析化学] TQ450.263[理学—化学]