摘要
应用固相萃取-超高效液相色谱-串联质谱法(SPE-UPLC-MS/MS)建立了测定地表水中的18种酰胺类除草剂的方法。水样经Oasis HLB固相萃取柱萃取,以丙酮-正己烷(3+7)混合液进行淋洗,洗脱液中加入内标物菲-D10后,在反相ACQUITY UPLCTMBEH C_(18)色谱柱上分离,以水-乙腈混合液为流动相进行梯度洗脱。质谱中选择电喷雾离子源和多反应监测模式。18种酰胺类除草剂的峰面积与其质量浓度在一定范围内呈线性关系,检出限(3S/N)在0.4~8.0ng·L^(-1)之间,测定下限(10S/N)在1.0~10ng·L^(-1)之间。加标回收率在80.1%~109%之间,测定值的相对标准偏差(n=6)在9.6%~15%之间。
An analytical method of UPLC-MS/MS combined with solid phase extraction（SPE）was developed for simultaneous determination of 18 amide herbicides in surface water.The samples were extracted on an Oasis HLB SPE column with a mixture of acetone and hexane as eluant.Phenanthrene-D10 used as the internal standard was added into the eluent.The analytes were separated on a reverse ACQUITY UPLCTMBEH C_（18） chromatographic column with a mixture of water and acetonitrile as the mobile phases for gradient elution.ESI and MRM were adopted in MS analysis.Linear relationships were found between the peak areas and the mass concentrations of 18 amide heribicides in defined ranges,with detection limits（3S/N）in the range of 0.4-8.0ng·L-1,and lower limits of determination in the range of 1.0-10ng·L-1.Recovery rates obtained by standard addition method were in the range of 80.1%- 109% and RSDs（n=6）were in the range of 9.6%- 15%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2016年第5期602-606,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
中国博士后科学基金项目(No.20080440374)
