香蕉及土壤中吡唑醚菌酯残留的高效液相色谱分析  

Determination of residual pyraclostrobin in banana and soil by HPLC

作　　者：赵方方[1] 谢德芳[1] 吕岱竹[1] 

机构地区：[1]中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室,海南海口571101

出　　处：《西北农林科技大学学报（自然科学版）》2016年第1期97-101,110,共6页Journal of Northwest A&F University(Natural Science Edition)

基　　金：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)

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。[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 ba- nana 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 a mount 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.

关 键 词：香蕉 土壤 吡唑醚菌酯 高效液相色谱 农药残留 

分 类 号：TQ450.263[化学工程—农药化工] S481.8[农业科学—农药学]