含脂羊毛中除虫脲和杀铃脲残留的高效液相色谱测定

Determination of Residual Diflubenzuron and Triflumuron in Greasy Wool by High-Performance Liquid Chromatography

建立了一套含脂羊毛中除虫脲和杀铃脲残留量的高效液相色谱测定方法．含脂羊毛样品（2g）在索氏提取器中用二氯甲烷提取约4h．提取液经预处理后在LC-Alumina-N小柱上固相萃取净化，以二氯甲烷／乙酸乙酯（体积比1：2）混合液为洗脱剂，色谱分析采用C18色谱柱，以乙腈／水（体积比41：59）作流动相，紫外检测波长254nm。方法的线性范围为0．05－10．0mg／L，除虫脲和杀铃脲在羊毛中的定量限都为0．1mg／kg．除虫脲和杀铃脲在1，2，4mg／kg3个水平上的平均加标回收率为79．9％－100．4％，回收率的相对标准偏差小于10％。

A high-performance liquid chromatographic method for the determination of diflubenzuron and triflumuron residues in greasy wool was developed. Wool samples （2 g） were extracted with diehloromethane in a Soxhlet extractor for about 4 h. After pretreatment, the extract was further cleaned-up by solid-phase extraction on an LC-Alumina-N cartridge using diehloromethane / ethyl acetate （ 1 ： 2, v/v） as the eluent. The analytes were separated on a C18 column by isocratic elution using acetonitrile/water （41： 59, v/v） as the mobile phase. The regression curves of both compounds were linear in the range of 0. 05-10. 0 mg/L. The quantification limits for diflubenzuron and triflumuron in wool were both 0. 1 mg/kg. Mean recoveries from wool samples fortified at 3 levels （1, 2 and 4 mg/kg） were 79. 9%~100. 4~ for diflubenzuron and triflumuron, with relative standard deviations lower than 10%.