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

作　　者：王玉健[1] 黄惠玲[1] 李华平 梁振纲 

机构地区：[1]海南出入境检验检疫局技术中心,海口570311 [2]海南利蒙特生物农药有限公司,海口570125

出　　处：《理化检验（化学分册）》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)

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%.

关 键 词：高效液相色谱-串联质谱法 三嗪类除草剂 水果 蔬菜 

分 类 号：O657.63[理学—分析化学]