摘要
应用高效液相色谱-串联质谱法测定果蔬中6种三嗪类除草剂(阿特拉津、扑草净、西玛津、莠灭净、扑灭津、西草净)的残留量。样品经乙腈提取,加N-丙基-乙二胺(PSA)固相吸附剂净化离心后,所得上清液供高效液相色谱-串联质谱分析。以Shiseido C_(18)色谱柱为固定相,以不同体积比混合的乙腈和0.02 mol·L^(-1)乙酸铵溶液为流动相做梯度洗脱,采用电喷雾正离子源模式多反应监测检测。6种三嗪类农药的质量浓度在20μg·L^(-1)以内与其峰面积呈线性关系,检出限(3S/N)均为0.005 mg·kg^(-1)。在0.008,0.02,0.04 mg·kg^(-1)3个浓度水平下进行回收试验,6种三嗪类农药的回收率在85.8%~97.8%之间,相对标准偏差(n=10)在3.6%~11%之间。
HPLC-MS/MS was applied to the determination of residual amounts of 6 triazine herbicides （i. e. , atrazine, prometryne, simazine, ametryn, propazine and sirnetryn） in fruils and vegetables. The sample was extracted with acetonitrile and purified by addition of PSA adsorbent. The supernatant was used for HPLC MS/MS analysis. Shiseido C18 column was used as stationary phase, and mixtures of acetonitrile and 0. 02 mol· L^-1 ammonium acetate solution mixed in different ratios were used as mobile phase in gradient elution. ESI^＋ as well as multi reactions monitoring was adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 6 triazine herbicides were obtained in the same range＇of 1-20μg·L^-1, with same detection limits （3S/N） of 0. 005 mg· kg^-1.Tests for recovery and precision were made by addition of 0. 008, 0. 02 and 0.04 mg· kg^-1 of mixed standard solution of the 6 triazine herbicides, giving values of recovery in the range of 85.8%-97.8% and values of RSD＇s（n=10）in the range of 3.6%-11%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2013年第10期1223-1227,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家质检总局科技计划项目(2013IK153)
海南省重点科技计划项目(ZDXM20120039
ZDXM20120040)
海南省自然科学基金(212018)
