摘要
[目的]建立了热带农业区水稻-辣椒轮作模式下辣椒种植季土壤中吡虫啉、啶虫脒与阿维菌残留同时快速检测方法。[方法]样品经乙腈-0.1%甲酸(V/V)提取、N-丙基乙二胺(PSA)与C_(18)混合分散剂净化,利用超高效液相色谱串联质谱(UPLC-MS/MS)与基质溶液匹配的外标法定量分析。[结果] 3种目标农药线性范围均超过3个数量级;3种添加质量分数(1.0、10.0、100.0μg/kg),土壤中3种农药平均回收率为63.7%～89.9%,相对标准偏差(RSD,n=3)为0.1%～13.6%;方法检出限(LOD,S/N=3)为0.06～0.26μg/kg,定量限(LOQ,S/N=10)为0.21～0.89μg/kg,均低于中国、欧盟辣椒中推荐最大残留限量值检测浓度。[结论]方法快速、简便、灵敏度高、重现性好,可满足实际检测需求。
[Aims] A simultaneous analysis method was optimized for the rapid determination of 3 kinds of pesticide residues in tropical soil under rice-vegetables rotation using QuEChERS-ultra-high performance liquid chromatographymass spectrometry(QuEChERS/UPLC-MS/MS). [Methods] The avermectin, imidacloprid and acetamiprid residues were effectively extracted with acetonitrile-0.1% formic acid(by vol), and then were simultaneously detected by external standard method after being purified with the mixed solid-phase dispersion of N-propylethylenedia-mine(PSA) and C18.[Results] The linear ranges were over 3 orders of magnitude for 3 kinds of pesticides. Under the three spiked levels of 1.0, 10.0 and 100.0 μg/kg, the average recoveries of the established method were 63.7-101.4%, with the relative standard deviation(RSD) of 0.1-13.6%(n=3). The limits of detection(LODs, S/N=3) of the established method were0.06-0.26 μg/kg, and also the limits of quantification(LOQs, S/N=10) were 0.21-0.89 μg/kg, which were all lower than concentration of the maximum residual limits for pepper recommended from China and UN. [Conclusions] The established method was rapid, easy operation, good sensitivity and reproducibility, could meet actual sample requirements for detection of pesticide residues.
作者
谭华东
张汇杰
武春媛
TAN Hua-dong;ZHANG Hui-jie;WU Chun-yuan(Environment and Plant Protection Institute,Chinese Academy of Tropical Agricultural Sciences,Haikou 571101,China;Danzhou Scientific Observing and Experimental Station of Agro-Environment,Ministry of Agriculture,Danzhou 571737, Hainan,China;School of Resources and Environment,Central China Agricultural University,Wuhan 430070,China)
出处
《农药》
CAS
CSCD
北大核心
2019年第1期45-49,共5页
Agrochemicals
基金
海南省重大科技计划(ZDKJ2017002)
中国热带农业科学院环境与植物保护研究所项目结余经费自主选题专项(hzsjy2018003)
关键词
QUECHERS
超高效液相色谱串联质谱法
农药残留
水稻-辣椒轮作
QuEChERS
ultra-high performance liquid chromatography tandem mass spectrometry
pesticide residues
rice-pepper rotation
