QuEChERS-高效液相色谱-串联质谱法检测甘薯和土壤中烯效唑残留的方法研究
Determination of Uniconazole Residue in Sweet Potatoes and Soil by QuEChERS-HPLC-MS/MS
左仁芳 1戴桂金 2王妙 3张玉涵 3罗杰 3熊浩 3刘志邦 3陈武瑛 3张卓3
作者信息
- 1. 凤凰县农业农村局植保植检站,湖南 凤凰 416200
- 2. 凤凰县农业农村局农业特色产业服务中心,湖南 凤凰 416299
- 3. 湖南省农业科学院植物保护研究所,湖南 长沙 410125
- 折叠
摘要
采用改良的QuEChERS方法进行前处理,建立了甘薯和土壤中烯效唑残留的QuEChERS-高效液相色谱-串联质谱检测方法.样品用含0.1%乙酸的乙腈振荡提取,经C18净化剂进行基质净化,采用C18反相色谱柱分离,进行LC-MS/MS检测.结果表明:烯效唑在0.000 5～1.0 mg/L浓度范围内,质量浓度与对应的峰面积间呈良好的线性关系,相关系数为0.995 1～0.995 9;在0.002、0.02、0.20 mg/kg 3个添加水平下,烯效唑在甘薯和土壤中的平均回收率为90.3%～106.7%,相对标准偏差为0.6%～3.6%,方法定量限为 0.002 mg/kg.该方法方便快捷、精准定量、检测灵敏,适用于甘薯和土壤样品中烯效唑的检测.
Abstract
A method for determining the uniconazole residue in sweet potatoes and soil was established by the combination of improved QuEChERS(quick,easy,cheap,effective,rugged,and safe)with high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Each sample was extracted by shaking with acetonitrile containing 0.1%(volume fraction)acetic acid,purified by C18 purification agent,separated by reversed-phase C18 column chromatography,and detected by LC-MS/MS.The results showed good linearity between the peak area and the uniconazole concentration within the range of 0.000 5-1.0 mg/L(R2 of 0.995 1-0.995 9).The recovery of uniconazole in sweet potatoes and soil at the spike levels of 0.002,0.02,and 0.20 mg/kg ranged from 90.3%to 106.7%with the relative standard deviations(RSDs)of 0.6%-3.6%.The established method showed the limit of quantification(LOQ)of 0.002 mg/kg.With easy operation,high sensitivity,and high accuracy,the established method is suitable for the detection of uniconazole in sweet potatoes and soil.
关键词
烯效唑/甘薯/高效液相色谱-串联质谱/残留/方法Key words
uniconazole/sweet potato/high-performance liquid chromatography-tandem mass spectrometry/residue/method引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据