超声辅助分散液液微萃取-高效液相色谱法测定蜂蜜中溴氰菊酯残留

Determination of deltamethrin residues in honey by HPLC coupled with ultrasound-assisted dispersive liquid-liquid microextraction

采用超声辅助分散液液微萃取技术结合高效液相色谱法测定蜂蜜中的溴氰菊酯。蜂蜜样品用乙腈∶水（1∶4,v/v）混合溶液提取,加入氯仿萃取,超声,离心,得到沉积相,进行HLPC分析。溴氰菊酯在10~1000μg/kg范围内线性良好,相关系数r=0.9998,富集倍数高达600倍。当蜂蜜样品的加标浓度为10、50、100μg/kg时,加标回收率为82.6%~97.3%,相对标准偏差为2.1%~3.8%。蜂蜜样品中溴氰菊酯的检出限为8μg/kg,定量限为40μg/kg。本方法具有简便快捷、准确灵敏、萃取效率高、有机溶剂消耗少等特点,可成功地应用于蜂蜜中溴氰菊酯残留的测定。

A method of HPLC combined with ultrasound-assisted dispersive liquid-liquid microextraction was used for the determination of deltamethrin in honey. The honey sample was extracted with mixed solution of acetonitrile∶water（1∶4,v/v）. After the chloroform extraction,ultrasound and centrifugation,sedimentary facies were determined by HPLC. Deltamethrin of 10~1000 μg/kg ranged with good linearity. The correlation coefficient was 0.9998,and the enrichment factor was up to 600. When the spiked concentration of honey samples came to 10,50,100 μg/kg,the recovery rates measured by standard addition method ranged from 82.6% to 97.3%,with the relative standard deviation（RSD） between 2.1% and 3.8%. The detection limit of deltamethrin in honey samples was 8 μg/kg,and the limit of quantification was 40 μg/kg. This method was simple and accurate,with high efficiency of extraction and little consumption of organic solvent. It could be successfully applied to the determination of deltamethrin residues in honey.