| 李广领, 郭梅燕, 谷珊山, 董丽红, 刘博, 郭文举, 陈锡岭*.花生植株、籽粒及田间土壤氟磺胺草醚残留分析方法研究[J].植物保护,2014,40(6):112-115. |
| 花生植株、籽粒及田间土壤氟磺胺草醚残留分析方法研究 |
| Residue analysis method of fomesafen in peanut plants, peanuts and peanut field soils by QuEChERS-HPLC |
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| DOI： |
| 中文关键词: 氟磺胺草醚 花生植株 花生籽粒 花生田土壤 基质分散萃取 残留分析 |
| 英文关键词:fomesafen peanut plant peanut peanut field soil dispersive solid phase extraction residues analysis |
| 基金项目:公益性行业(农业)科研专项(201203098); 国家级大学生创新创业训练计划项目(20121046701703); 河南省教育厅科学技术研究重点项目(13B210003) |
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| 中文摘要: |
| 在前人研究基础上, 确立了花生植株以甲醇、乙二胺-N-丙基硅烷（PSA）和石墨化炭黑（GCB）为基质分散萃取材料, 花生籽粒和田间土壤分别以酸化甲醇和乙腈为分散萃取溶剂, 以PSA为基质净化材料的3类氟磺胺草醚残留样品前处理程序, 建立并优化了花生籽粒、花生植株和田间土壤氟磺胺草醚残留高效液相色谱检测方法。结果显示, 氟磺胺草醚在0.05~10.0 mg/L质量浓度范围内与对应色谱峰积分面积线性响应良好, 回归方程为 y =2.562 8x -0.006 8（r2=0.999 8）。在0.05 ~0.5 mg/kg氟磺胺草醚添加范围内, 花生籽粒、植株和田间土壤中的平均回收率为85.6%~113.5%, 相对标准偏差为1.5%~9.7%。花生植株、籽粒和田间土壤中氟磺胺草醚的检出限分别为0.024、0.029和0.031 mg/kg。基质效应试验结果表明, 该样品前处理方法获得的分析样品基质效应不明显, 表明该残留样本前处理方法和样品检测方法简便、高效、经济、可靠, 可满足氟磺胺草醚在花生植株、籽粒及田间土壤中残留的定量检测要求。 |
| 英文摘要: |
| A method has been developed for determining fomesafen residues in peanut plants, peanuts and peanut field soil by high performance liquid chromatography (HPLC). Fomesafen residues in peanut plants was extracted by methanol and then purified by primary secondary amine (PSA) and graphitized carbon black (GCB), and fomesafen residues in peanuts or soil was extracted by methanol or acetonitrile (containing 1% formic acid), and then purified by PSA. Then these detection samples were detected by HPLC under the optimal conditions. The results showed, under the optimal conditions, the calibration curves showed good linearity(y = 2.562 8x -0.006 8, r2=0.999 8) at 0.05-10.0 mg/L concentration of fomesafen, the average recoveries of fomesafen in peanut plants, peanuts, peanut field soil at the three spiked concentration levels ranged from 85.6% to 113.5%, and the relative standard deviations was 1.5%-9.7%. The lowest concentration detected of fomesafen in peanut plants, peanuts and peanut field soil were 0.024 mg/kg, 0.029 mg/kg and 0.031 mg/kg, respectively. The matrix effect of the method was studied and there was no significant difference. In sum, the method was simple, efficient, economy and reliable, which can meet quantitative detection requirements in peanut, peanut plants and soil. |
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