高级检索

    高效液相色谱-串联质谱法测定果蔬中6种三嗪类除草剂的残留量

    HPLC-MS/MS Determination of Residual Amounts of 6 Triazine Herbicides in Fruits and Vegetables

    • 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 C18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20 μg·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。

       

      Abstract: HPLC-MS/MS was applied to the determination of residual amounts of 6 triazine herbicides (i.e., atrazine, prometryne, simazine, ametryn, propazine and simetryn) in fruits 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 1-20 μg·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%.

       

    /

    返回文章
    返回