摘要
建立了柱前衍生化超高效液相色谱-串联质谱(UPLC-MS/MS)检测水体中代森锰锌残留的分析方法。样品在碱性条件下用EDTA溶液配位反应后,以碘甲烷进行柱前衍生化,以Cleanrt■-PEP固相萃取柱进行富集浓缩和净化,结合UPLC-MS/MS检测,外标法定量。检测结果表明,代森锰锌在10~1000 ng/L浓度范围内线性关系良好,线性相关系数R2=0.9991;在10 ng/L、100 ng/L和1000 ng/L三个添加水平下,平均回收率在79.2%~101.5%范围内,相对标准偏差(RSDs,n=5)在2.1%~6.9%之间;定量限为10 ng/L。该方法具有灵敏度高、稳定性好和准确度高等优点,将方法应用于泰安市区周围河流和水库水体检测,检测结果显示均未超标。方法适用于水体中痕量代森锰锌检测。
An analytical method for the determination of trace mancozeb residues in water by pre-column derivatization ultra-high performance liquid-tandem mass spectrometry(UPLC-MS/MS) was established.After coordination reaction with EDTA solution under alkaline conditions,the sample was pre-column derivated with iodide methane,then purified and enriched with Cleanrt■-pep phase extraction column,detected with UPLC-MS/MS,and quantified by external standard method.The results showed that good linearity was achieved at the concentration levels of 10 ng/L-1 000 ng/L,with the linear correlation coefficient(R^2) of 0.999.The average recoveries of 79.2%-101.5% were obtained at three concentration levels of 10,100 and 1 000 ng/L,and the relative standard deviations(RSDs,n=5) were 2.1%-6.9%.The quantitation limit was 10 ng/L.The method has the advantages of high sensitivity,good stability and high accuracy.The method has been applied to the detection of mancozeb in rivers and reservoirs around Tai’an City.The test results showed that they were not exceeded.The method is applicable to the detection of trace mancozeb in water.
作者
杨松
柏杨
王文利
许乐园
高云
王苓
邹楠
慕卫
YANG Song;BAI Yang;WANG Wenli;XU Leyuan;GAO Yun;WANG Ling;ZOU Nan;MU Wei(College of Plant Protection,Shandong Agricultural University,Tai’an 271018;Research Center of Pesticide Environmental Toxicology,Shandong Agricultural University,Tai’an 271018)
出处
《分析科学学报》
CAS
CSCD
北大核心
2020年第3期385-389,共5页
Journal of Analytical Science
基金
国家自然科学基金(No.31772203)。
关键词
超高效液相色谱-串联质谱
代森锰锌
水体
残留
Ultra-high performance liquid chromatography-tandem mass spectrometry
Mancozeb
Water body
Residue
