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

涪陵出入境检验检疫局

基金项目:

涪陵区科技计划项目(FLKJ,2016ABB1052)；

详细信息

作者简介:
郑洋 (1989-) , 男, 硕士研究生, 工程师, 主要从事食品安全检测分析方面的研究, E-mail:651192869@qq.com。;

中图分类号: O657.72;TQ450.263
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出版历程
- 收稿日期: 2017-02-22

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

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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。
- 氯吡苯脲 /
- 土壤 /
- 固相萃取 /
- 超高效液相色谱法
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.
- forchlorfenuron /
- soil /
- solid-phase extraction /
- ultra performance liquid chromatography

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