液面悬浮单滴微萃取—高效液相色谱法测定果汁中两类农药残留

Determination of two kinds of pesticide residues in peach juice drink by floated organic drop microextraction-high performance liquid chromatography

采用悬浮单液滴微萃取-高效液相色谱法测定葡萄果汁中氨基甲酸酯和苯甲酰脲两类农药残留。采用Diamonsil C18(5μm,250mm×4.6mmi.d.)柱,乙腈:甲醇:水(体积比18:70:12)流动相,流速1.0mL/min,室温,检测波长240nm。最佳萃取条件:8μL正十二醇液滴为萃取剂,40℃,转速420r/min,pH=4,NaCl含量30g/L,时间25min。西维因、抗蚜威、除虫脲、氟铃脲和氟苯脲在0.01～10.0mg/L范围内均有良好线性,检出限在0.005～0.01mg/L之间,添加回收率在88.49%～101.86%之间,相对标准偏差(RSD)为1.99%～3.47%。

A method of floated organic drop microextraction （FDME）-high performance liquid chromatography （HPLC） was developed for extraction and determination of 2 kinds of pesticide residues from peach juice drink samples.The components were separated by a Diamonsil C,, （5μm,250mm × 4.6mm i.d.）.Mobile phase was a mixture of acetonitrile, methanol and water （the ratio of volume was 18：70： 12）. Factors relevant to the extraction efficiency were studied and optimized. The optimized extraction conditions： extraction solvent： 1- dodecanol; extraction temperature ：40%; sodium chloride concentration ： 30g/L; pH = 4; microdrop volumes ： 8μL; stirring rate： 420r/min and the extraction time ：25min.The methodology exhibited good linearity between 0.01-10.0mg/mL with correlation coefficiency of 0.9999.The detection limits of quantification were 0.005-0.01mg/L.The average recovery of pesticides ranged from 88.49% to 101.86%.The relative standard deviations （RSD） were 1.99%-3.47% （n =6）.