高效液相色谱法测定蔬菜中除虫脲、灭幼脲和杀铃脲残留

Determination of Diflubenzuron,Chlorbenzuron and Triflumuron Residue in Vegetables by HPLC

建立高效液相色谱测定蔬菜中除虫脲、灭幼脲和杀铃脲残留的检测方法.蔬菜样品用乙腈提取,经DisQuE 分散固相萃取试剂盒净化,C18 色谱柱（250 mm×4.6 mm,5 μm） 分离,以乙腈– 水（68∶32）溶液洗脱,二极管阵列（PDA） 检测器检测,外标法定量.在0.02～1.0 mg/L 范围内,除虫脲、灭幼脲和杀铃脲的质量浓度与对应的色谱峰面积线性相关,除虫脲和灭幼脲的检出限为0.010 mg/kg,杀铃脲的检出限为0.015 mg/kg.除虫脲、灭幼脲和杀铃脲标准溶液的色谱峰面积的日内相对标准偏差分别为1.03%,1.31%,0.82%（n=6）,日间相对标准偏差分别为1.43%,1.56%,1.06%（n=6）.加标回收率为88.7%～108.0%.该方法简单、快速、准确,适合蔬菜中除虫脲、灭幼脲和杀铃脲残留的测定.

HPLC method was established for determination of diflubenzuron, chlorbenzuron and triflumuron residue in vegetables. The samples were extracted with acetonitrile and purified by Dis Qu E dispersive solid-phase extraction kit, and then, it was separated on a C_(18) column(250 mm×4.6 mm, 5 μm) with mobile phase of acetonitrile–water(68∶32) solution, diode array was used as a detector to collect signals, the quantification was determined by external standard method. There was a linear relationship between chromatographic peak area and concentration for diflubenzuron, chlorbenzuron and triflumuron at the range of 0.02–1.0 mg/L, the detection limit of diflubenzuron and chlorbenzuron was 0.010 mg/kg, the detection limit of triflumuron was 0.015 mg/kg. The inner-day RSD of peak area for the standard solution of diflubenzuron, chlorbenzuron and triflumuron were 1.03%, 1.31%, 0.82%(n=6), respectively. The intra-day RSD of peak area for the standard solution of diflubenzuron, chlorbenzuron and triflumuron were 1.43%, 1.56%, 1.06%(n=6), respectively. The range of recovery rate were 88.7%–108.0%. The method was simple, rapid, accurate and suitable for determination of diflubenzuron, chlorbenzuron and triflumuron residue in vegetables.