摘要
[目的]建立了基于多壁碳纳米管净化,超高效液相色谱-飞行时间质谱技术同时测定香草兰中13种农药残留的分析方法。[方法]香草兰样品采用乙腈提取后,经多壁碳纳米管净化,超高效液相色谱-飞行时间质谱测定。[结果]嘧菌酯等13种农药的质量浓度在0.0005～0.2 mg/L范围内线性关系良好,最低检出限在1.5～3μg/kg之间,相关系数均大于0.99,平均加标回收率在77.92%～119.10%之间,相对标准偏差在0.55%～17.70%之间。与N-丙基乙二胺吸附剂相比,多壁碳纳米管具有更好的净化性能。[结论]方法学考察和实际样品的测定证明该方法具有简便、快速、准确度高等优点,可用于香草兰中嘧菌酯等13种农药的检测。
[Aims]A method was developed for the simultaneous determination of 13 pesticides in vanilla by using ultra-performance liquid chromatography coupled with time of flight mass spectrometry (UPLC-TOF/MS). [Methods]The vanilla samples were extracted with acetonitrile and cleaned up with multiwalled carbon nanotubes, then determined by UPLC-TOF/MS.[Results]The limits of detection (LOD)for 13 pesticides ranged from 1.5to 3μg/kg.Calibration curves exhibited good linearity relation over the concentration range from 0.0005 to 0.2mg/L, with their correlation coefficients above 0.99.Average recoveries for 13 pesticides ranged from 77.92 to 119.10%,with relative standard deviations (RSD)ranged from 0.55 to 17.70%.Compared with primary secondary amine sorbent,the multiwalled carbon nanotubes has better purification performance.[Conclusions]The results of method validation and real sample determination demonstrate that the developed method was sensitive,rapid and accurate.As a result,it can be applied for determination of 13 pesticides in vanilla.
作者
乐渊
马晨
黎舒怀
李春丽
LE Yuan;MA Chen;LI Shu-huai;LI Chun-li(Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables,Analysis and Testing Center,Chinese Academy of Tropical Agricultural Sciences,Haikou 571101,China)
出处
《农药》
CAS
CSCD
北大核心
2018年第12期895-900,共6页
Agrochemicals
基金
中国热带农业科学院基本科研业务费专项(1630082016003)
热带农产品质量安全科技创新团队项目(1630082017002)
关键词
香草兰
农药残留
多壁碳纳米管
超高效液相色谱
飞行时间质谱
vanilla
pesticide residues
multiwalled carbon nanotubes
ultra-performance liquid chromatography
time of flight mass spectrometry
