高效液相色谱法测定柑橘和土壤中残留的多菌灵

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。

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

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.