色谱

色谱

• 研究论文 • 上一篇    下一篇

高效液相色谱法测定柑橘和土壤中残留的多菌灵

沈菁1*, 刘军1, 刘建2   

  1. 1.Agricultural Testing & Information Center, Hubei Academy of Agriculture Science, Wuhan 430064, China; 2.Hubei Province Key Laboratory of Biotechnology of Traditional Chinese Medicine, Hubei University, Wuhan 430062, China
  • 收稿日期:2008-09-22 修回日期:2008-11-21 出版日期:2009-05-30 发布日期:1982-09-25
  • 通讯作者: 沈菁

Determination of carbendazim residue in orange and soil using high performance liquid chromatography

SHEN Jing1*, LIU Jun1, LIU Jian2   

  1. 1.Agricultural Testing & Information Center, Hubei Academy of Agriculture Science, Wuhan 430064, China; 2.Hubei Province Key Laboratory of Biotechnology of Traditional Chinese Medicine, Hubei University, Wuhan 430062, China
  • Received:2008-09-22 Revised:2008-11-21 Online:2009-05-30 Published:1982-09-25
  • Contact: SHEN Jing

PDF

767

被引次数

40

摘要： 建立了柑橘和土壤中多菌灵残留量的高效液相色谱(HPLC)分析方法。柑橘果肉、果皮、全果和土壤样品中残留的多菌灵用碱性乙腈溶液提取,经NH2固相萃取(SPE)柱净化,HPLC分离,紫外检测器检测,外标法定量。在0.02～5.0 mg/L范围内,多菌灵的峰面积与其质量浓度呈良好的线性关系,相关系数为0.9997。柑橘果肉、果皮、全果和土壤中添加0.05～0.5 mg/kg多菌灵标准品的平均回收率为89.2%～102%,相对标准偏差为1.8%～9.1%;柑橘果肉和土壤中多菌灵的最低检测浓度为0.05 mg/kg,柑橘果皮和全果中多菌灵的最低检测浓度为0.1 mg/kg。该方法的灵敏度、准确度和精密度均符合农药残留测定的技术要求。

关键词: 多菌灵残留, 柑橘, 高效液相色谱法, 固相萃取, 土壤

Abstract: An analytical method of high performance liquid chromatography (HPLC) was established for determining carbendazim residue in orange and soil. The residue was extracted with alkaline acetonitrile, cleaned-up by NH2 solid-phase extraction (SPE), separated on a Luna C18 column (250 mm×4.6 mm, 5 μm) using 10 mmol/L ammonium acetate solution (A) and acetonitrile (B) as the mobile phases with the gradient elution (0→15 min, 20%B; 15→25 min, 80%B; 25→35 min, 20%B) at a flow rate of 1.0 mL/min, and detected at 275 nm. The method showed a linear relationship between peak area and concentration at the range of 0.02~5.0 mg/L for carbendazim. The average recoveries of the method ranged from 89.2% to 102% with the relative standard deviations of 1.8%~ 9.1% at spiked level of 0.05~ 0.5 mg/kg. The limit of detection was 0.05 mg/kg in sarcocarp and soil, and that was 0.1 mg/kg in pericarp and whole orange. The method is characterized by simplicity, higher sensitivity and accuracy.

Key words: carbendazim residue, orange, soil , solid-phase extraction (SPE), high performance liquid chromatography (HPLC)