摘要
[目的]采用超高液相色谱-三重四级杆复合线性离子阱质谱(UPLC-Q-TRAP-MS)技术,结合加速溶剂萃取(ASE)前处理技术,建立土壤中23种除草剂残留的快速筛查确证方法。[方法]干燥研磨后的土壤样品用硅藻土混合分散,以丙酮-二氯甲烷(体积比1∶1)为萃取剂,经ASE萃取富集,N-丙基乙二胺(PSA)、C_(18)吸附剂、无水MgSO_4净化后,经BEH C_(18)色谱柱分离,甲醇-0.1%甲酸梯度洗脱,采用多反应监测-信息关联采集-增强子离子扫描(MRM-IDA-EPI)模式检测,外标法定量。[结果]23种待测物在0.5~500μg/L范围内线性关系良好;方法定量限(S/N=10)为0.2~1.5μg/kg;添加水平为定量限、2倍定量限、10倍定量限时,平均回收率为75.91%~105.22%之间,相对标准偏差为1.77%~10.21%。[结论]方法前处理过程简单,净化效果好,灵敏度高,适用土壤中除草剂的快速筛查和确证分析。
[Aims] A rapid screening and confirmatory analysis method for 23 herbicides in soil by unltra performance liquid chromatography-tandem mass spectrometry with linear trap（UPLC-Q-TRAP） combined with accelerated solvent extraction（ASE）.[Methods] After mixing soil and diatomite,the sample was extracted by ASE with the mixture of acetone and dichloromethane（1 ∶1,by vol） as extraction solvent.The extract was purified by mixture of primary secondary amine（PSA）,octadecyl（C18） and unhydrous magnesium sulfate（MgSO4）.Purified extract was separated by BEH C18 column,with the mobile phase of methanol and water（0.1% formic acid） by gradient elution.[Results] The23 herbicides were detected under multi reaction monitoring（MRM）-information dependent acquisition（IDA）-enhanced product ion（EPI） scan mode.External standard method was used in quantitative method.The results showed that the ratio of peak area of 23 herbicides versus their concentration had a good linearity in the range of 0.5-500 μg/L.The limited of quantitate（LOQ） ranged from 0.2 to 1.5 μg/kg.As spiking amount is LOQ,2×LOQ and 10×LOQ,the recoveries of standard spiking of 23 herbicides were 75.91-105.22% with the relative standard deviations was1.77-10.21%.[Conclusions] This method has simple sample preparation,good purification effect and high sensitivity,which is suitable for rapid screening and confirmatory analysis of herbicides in soil.
作者
孟繁磊
魏春雁
蔡红梅
张振都
何智勇
张奇
宋志峰
MENG Fan-lei;WEI Chun-yan;CAI Hong-mei;ZHANG Zhen-du;HE Zhi-yong;ZHANG-Qi;SONG Zhi-feng(Institute of Agricultural Quality Standard and Testing Technology,Jilin Academy of Agricultural Sciences,Changchun 130033,China)
出处
《农药》
CAS
CSCD
北大核心
2018年第7期516-519,526,共5页
Agrochemicals
基金
吉林省农业科技创新工程项目(CXGC2017ZY037)
