通过对加速溶剂莘取(ASE)条件、固相萃取小柱净化(SPE)条件和高效液相色谱(HPLC)仪器分析条件进行优化,建立了“ASE提取-SPE净化-HPLC分析”同时测定土壤中西玛津、莠去通、西草净、莠去津、仲丁通、扑灭通、莠灭净、扑灭津、特丁津、扑灭净、去草净共11种三嗪类除草剂残留量方法.土壤样品经丙酮:二氯甲烷(1:1)提取,提取液浓缩后经固相萃取小柱净化,高效液相色谱法-二极管阵列检测器(DAD)测定,外标法定量.11种三嗪类除草剂在0.05-5.0 mg· L-1范围内线性良好,相关系数在0.9998-0.9999之间.方法检出限在2.0× 10-3-4.1×10-3 mg· kg-1之间,对实际土壤进行高、中、低浓度分别为500.0、100.0、20.0 μg·kg-1的加标测定,平行分析(n=6)的相对标准偏差(RSD)均在15％以内,三嗪类除草剂回收率在62.7％-100.1％之间.该方法能够满足土壤中多种三嗪类除草剂残留量的检测需要.
An analytical method was developed for the determination of 11 triazine pesticides in soil by high performance liquid chromatography (HPLC)with accelerated solvent extraction (ASE) and solid phase extraction (SPE) column purification.The factors such as instrumental conditions of ASE,conditions for SPE purification and chromatographic conditions were optimized.In this study,the soil samples were extracted with acetone:dichloromethane (1:1) using ASE,enriched and then cleaned up with SPE column.The HPLC analysis followed by diode array detector (DAD)was performed,and quantitative analysis was conducted by the external standard method.The results showed that the 11 triazine herbicides were effectively separated using the above method.The linear regression analysis data indicated that there was a good linear relationship between response and concentration in the range 0.05-5.0 mg·L-1,and the correlation coefficients were 0.9998-0.9999.The limits of detection(LOD) of this method ranged from 2.0× 10-3 to 4.1 × 10-3 mg· kg-1.The method was also validated by analyzing spiked soil samples at three levels(500.0,100.0 and 20.0 μg·kg-1).The average recoveries of the 11 triazine herbicides in spiked soils ranged from 62.7％ to 100.1％,the relative standard deviations (RSD)were all within 15％.The performance of the method was further validated by analysis of regional soil sample.Similarly,the overall results confirmed that the analytical method could meet the requirements for the simultaneous determination of 11 triazine herbicides residues in soil.
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