固相萃取-超高效液相色谱法测定土壤中氯吡苯脲的残留

郑洋; 吴杰; 唐璜; 王安良; 杨文友; 徐亚琴; 郭禹良

doi:10.13386/j.issn1002-0306.2017.18.050

固相萃取-超高效液相色谱法测定土壤中氯吡苯脲的残留

Residue determination of forchlorfenuron in soil by solid-phase extraction and ultra performance liquid chromatography

摘要

摘要: 采用固相萃取-超高效液相色谱法（SPE-UPLC）快速测定土壤中的氯吡苯脲残留量,对比确定了合适的前处理方法,并系统优化了测定方法中的提取和净化条件。实验结果表明:当采用乙腈提取,超声时间为30 min,离心转速为5000 r/min,PSA柱净化,色谱流动相为:V乙睛∶V水=65∶35时土壤中氯吡苯脲的提取效果最佳。氯吡苯脲在0.05⁵.0μg/m L质量浓度范围内与峰面积呈良好的线性关系（r=0.9999）,定量限为0.025 mg/kg,氯吡苯脲的添加回收率为78.34%¹02.4%,相对标准偏差为3.24%⁶.65%。该方法测定速度快,准确度和精密度符合农药残留分析,能够满足对土壤中氯吡苯脲残留的快速测定要求。

Abstract: The forchlorfenuron residues in soil were determined quickly by solid-phase extraction and ultra performance liquid chromatography ( SPE-UPLC) in this paper. And this paper compared to determine the appropriate pre-treatment methods, optimized the extraction method and purification conditions.The optimal conditions were obtained that the sample was extracted with acetonitrile for 30 min by ultrasonic method, centrifuged in 5000 r/min and cleaned up with the PSA column.Forchlorfenuron was determined by ultra performance liquid chromatography using acetonitrile-water ( 65 ∶ 35) as mobile phase.The developed method showed a good linear relationship in the range of 0.05 ~ 5.0 μg/m L for forchlorfenuron, with correlation coefficient of 0.9999.The limit of quantitation for forchlorfenuron was 0.025 mg/kg. The average recovery rates were78.34% ¹02.4%, with relative standard deviation ( RSD) ranging from 3.24% to 6.65%.The method is fast, highly sensitivity, repeatable and suitable for the determination of forchlorfenuron residues in soil.