| 摘要: |
| 【目的】建立吡唑醚菌酯在香蕉和土壤中残留量的高效液相色谱检测方法。【方法】用乙腈提取试样，分别采用Strata/NH2和Carbon/NH2固相萃取柱对香蕉中吡唑醚菌酯进行净化，对2种SPE柱进行对比，并优化其色谱条件，采用高效液相色谱 紫外检测器进行测定。【结果】香蕉加标样品中，2种SPE柱均可与杂质较好分离；Carbon/NH2柱净化后杂质峰较少，但是目标物响应值明显降低，回收率仅为35.5%，而Strata/NH2柱净化后，回收率达到95%以上，因此选择Strata/NH2柱净化。在添加量为0.01～0.1 mg/kg时，吡唑醚菌酯在香蕉全蕉中的平均回收率为82%～96%，相对标准偏差为1.7%～2.7%；在蕉肉中的平均回收率为82%～96%，相对标准偏差为1.3%～2.7%；在土壤中的平均回收率为81%～96%，相对标准偏差为0.9%～2.2%。该方法的最低检出量为1×10-10 g，最低检出浓度为0.01 mg/kg。【结论】该方法灵敏度和准确度高，检测限低，完全满足香蕉和土壤中吡唑醚菌酯残留量的检测要求。 |
| 关键词: 香蕉 土壤 吡唑醚菌酯 高效液相色谱 农药残留 |
| DOI： |
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| 基金项目:农业部农药残留试验项目(2013F285)；中国热带农业科学院分析测试中心主任基金项目（2013-01） |
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| Determination of residual pyraclostrobin in banana and soil by HPLC |
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ZHAO Fang-fang,XIE De-fang,LÜ Dai-zhu
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| Abstract: |
| 【Objective】An analysis method for pyraclostrobin detection in banana and soil by HPLC (High performance liquid phase chromatography) was established.【Method】Samples were extracted with acetonitrile and cleaned up using the Strata/NH2 and Carbon/NH2 SPE columns.The results with the two solid phase extraction columns were compared and the chromatographic conditions for pyraclostrobin in banana and soil were optimized before samples were injected to the HPLC-UV (High performance liquid phase chromatography-Ultra-violet detector) for analysis.【Result】Pyraclostrobin and impurity had better separation with the two SPE columns in the spiked samples.The impurity was less but the target response decreased (the value of recovery was 35.5%) with Carbon/NH2 SPE column.The values of recovery were higher than 95% with Strata/NH2 SPE column.Thus,Strata/NH2 SPE column was selected.Values of RSD,S in the whole fruit were 1.7%-2.7%,and values of recovery were 82%-96% with additive amount of 0.01-0.1 mg/kg.Similarly,values of RSD,S in flesh were 1.3%-2.7% and values of recovery were 82%-96%.Values of RSD,S in soil were 0.9%-2.2% and values of recovery were 81%-96%.The detection limit of this method for pyraclostrobin was 1×10-10 g and the quantitation limit was 0.01 mg/kg.【Conclusion】The method could be used to detect pyraclostrobin in banana and soil due to its high sensitivity,high accuracy and low detection limit. |
| Key words: banana soil pyraclostrobin HPLC pesticide residue |
