摘要
建立一种测定土壤中5种三唑类农药残留的超高效液相色谱-四级杆-静电场轨道阱高分辨质谱检测方法。样品用乙腈超声提取,抽滤,浓缩,正己烷定容,采用Thermo Hypersil GOLD色谱柱(100 mm×2.1 mm,1.9μm)分离,以甲醇和0.1%甲酸5 mmol·L^(-1)乙酸铵的水溶液进行梯度洗脱,在全扫描(Full MS)-数据依赖二级扫描(dd-MS 2)模式下进行检测。该方法利用物质的精确分子量、相对保留时间、同位素丰度比例等指标对农药残留微量成分进行快速、准确的定性检验。方法的平均加标回收率范围为75.5%~98.5%,RSD为0.89~4.56%,5种三唑类农药检测限范围为0.01~1 mg·L^(-1)。该方法的建立为土壤中丙硫唑、苯醚甲环唑、丙环唑、腈菌唑、多效唑5种三唑类农药残留的检测提供了参考。
The aim was to establish a determining method of five trizole pesticides residues in soil by ultra performance liquid chromatography-quadrupole orbitrap high resolution mass.The samples were ultrasonically extracted with acetonitrile,suction filtered,concentrated,and the volume was adjusted with n-hexane.The samples were separated by Thermo Hypersil GOLD column(100 mm×2.1 mm,1.9μm) using a binary solvent system composed of methanol and water(0.1%formic acid and 5 mmol·L^(-1)ammonium acetate)by gradient elution.The analytes were determined by quadrupole-orbitrap high resolution mass spectrometry in full-MS and data-dependent scan(ddMS 2)mode.The method can quickly and accurately qualitatively test the trace components of pesticide residues by using the accurate molecular weight,relative retention time,isotope abundance ratio and other indexes.Average recoveries of five trizole bactericides ranged from 75.5%to 98.5%,with the relative standard deviations between 0.89%and 4.56%.The detection limits of five trizole pesticides residues ranged from 0.01 mg·L^(-1)to 1 mg·L^(-1).The establishment of method in this study provides reference for the detection of five trizole pesticides residues in soil,including prothioconazole,difenoconazole,propiconazole,myclobutanil,paclobutrazol.
作者
赵增兵
孔维刚
成兰兴
柴勇利
陈波
杨舒程
侯占峰
ZHAO Zeng-bing;KONG Wei-gang;CHENG Lan-xing;CHAI Yong-li;CHEN Bo;YANG Shu-cheng;HOU Zhan-feng(Henan Chemical Industry Research Institute Co.,Ltd.,Zhengzhou 450052,China;Physical Evidence Appraisal Center,Zhengzhou Public Security Bureau,Zhengzhou 450000,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2021年第2期387-392,共6页
Chemical Research and Application
基金
河南省科学院助推科技成果转化专项项目(190208008、200208003)资助
河南省科学院基本科研费项目(200608038)资助。
关键词
三唑类农药
超高效液相色谱
静电场轨道阱
高分辨质谱
土壤
trizole pesticides
ultra high performance liquid chromatography
orbitrap
high resolution mass
soil
