高效液相色谱法测定马铃薯和土壤中的辛硫磷残留

Determination of phoxim residues in potato and soil by high performance liquid chromatography

中文关键词:  辛硫磷  马铃薯  残留  土壤

英文关键词:phoxim  potato  residue  soil

中文摘要:

      目的 建立高效液相色谱法测定马铃薯和土壤中辛硫磷残留的分析方法。方法 样品经乙腈萃取, 氨基固相萃取小柱净化, 采用以色谱柱Agilent ZARBAX SB-C18柱(4.6 mm×250 mm, 5 μm)分离, 甲醇/水(75:25, V:V)为流动相等度洗脱后紫外检测器检测, 检测波长为280 nm。结果 辛硫磷在0.05~10 mg/L浓度范围内线性关系良好(r2=0.9990); 最低检出限为0.02 mg/kg, 辛硫磷在马铃薯块茎、植株和土壤中的添加水平为0.05~5.0 mg/kg时, 添加回收率分别为92.3%~102.4%、98.5%~109.1%和89.7%~104.3%, 相对标准偏差分别为1.0%~2.5%、1.4%~5.6%和1.4%~2.1%。结论 该方法具有快速、准确、灵敏度高等特点, 符合国家标准对食品中农药残留测定的要求。

英文摘要:

      Objective To establish a method for determination of phoxim residues in potato and soil by high performance liquid chromatography (HPLC). Methods Phoxim residues were extracted from potato and soil with acetonitrile, then purified with NH2 solid phase extraction (SPE) column, and separated by Agilent ZARBAX SB-C18 column (4.6 mm×250 mm, 5 μm) using a mixture of methanol and water (75:25, V:V) as mobile phase for isocratic elution. The ultraviolet detection wavelength was set at 280 nm．Results Phoxim had a good linear relationship in the concentration range of 0.05~10 mg/L (r2=0.9990) and the limit of detection was 0.02 mg/kg. The average recoveries of phoxim spiked at 0.05~5.0 mg/kg were 92.3%~102.4% for potato tuber, 98.5%~109.1% for potato shoots and 89.7%~104.3% for soil, respectively, with relative standard deviations (RSDs) of 1.0%~2.5%, 1.4%~5.6% and 1.4%~2.1%, respectively in potato tuber, shoots and soil. Conclusion The established method is rapid, accurate and sensitive, which can meet the national standard requirements for pesticide determination.