加速溶剂提取-固相萃取净化-高效液相色谱法测定土壤中12种三嗪类除草剂的残留量

Determination of Twelve Triazine Herbicide Residues in Soil by High Performance Liquid Chromatography with Accelerated Solvent Extraction and Solid-phase Extraction

建立了加速溶剂（ASE）提取一固相萃取（SPE）净化一高效液相色谱（HPLC）同时检测土壤中12种三嗪类除草剂残留量的方法。土壤样品经过乙腈提取，氨基（NH：）固相萃取柱净化，高效液相色谱法一二极管阵列检测器（DAD）测定，外标法定量。12种三嗪类除草剂在0．02~2．00mg·L。范围内线性关系良好，相关系数在O．9984~0．9999之间，方法检出限在0．004~0．005mg·kg。之间。在0．02、0．04和0．10mg·kg。3个浓度水平，平均添加回收率在75．2％-112．7％之间，RSD值在1．1％-13．3％之间，方法定量限在0．01~0．02mg·kg。之间。该方法可以满足土壤中多种三嗪类农药残留量的检测。

A method was established by high performance liquid chromatography（HPLC ） coupled with accelerated solvent extraction （ASE） and solid-phase extraction（SPE ） for determination of 12 triazine herbicides residues in soil samples. In this study, the samples were ex- tracted with acetonitrile using ASE, enriched and then cleaned up with NH2 solid-phase extraction cartridge. The HPLC analysis followed by diode array detector（ DAD ） was performed using a C18 column, and quantitative analysis was conducted by the external standard method. The results showed that 12 triazine herbicides were effectively separated using the method above. The linear regression analysis da- ta indicated that there was a good linear relationship between response and concentration in the range 0.02~2.00 mg-L-1, and the correlation coefficients were 0.998 4-0.999 9. The limits of detection（ LOD ） of this method ranged from 0.004 to 0.005 rag-kg-1. The method was also validated by analyzing spiked soil samples at the three levels（0.02, 0.04 and 0.10 rag-kg-1 ）. The average recoveries of 12 triazine herbicides in spiked soils were ranged from 75.2% to 112.7% with the relative l standard deviations （RSD） between 1% and 13.3%, and the limits of quantity （LOQ） were in the range of 0.01- 0.02 rag＂ kg-1. The performance of the method was further validated by analysis of two different regional soil samples. Similarly, the overall results confirmed that the analytical method could meet the requirements for the si- multaneous determination of 12 triazine herbicides residues in soil.