高效液相色谱法同时测定含脂羊毛中残留的除虫脲和杀铃脲

建立了同时测定含脂羊毛中除虫脲和杀铃脲的反相高效液相色谱方法。样品用正己烷-乙醚混合溶剂提取,经凝胶渗透色谱柱和固相萃取柱净化后,采用反相高效液相色谱-二极管阵列检测器检测,外标法定量。除虫脲和杀铃脲分别在0.41～41 mg/L和0.38～38 mg/L范围内线性关系良好,相关系数分别为0.9996和0.9999。最低检出限:除虫脲为0.22 mg/kg,杀铃脲为0.18 mg/kg;最低定量限:除虫脲为0.73 mg/kg,杀铃脲为0.60 mg/kg。在添加水平为0.76～10.25 mg/kg的除虫脲和杀铃脲时,平均加标回收率为86.3%～96.7%,相对标准偏差为4.2%～8.7%。该方法杂质干扰小、回收率高、重现性好,能够对含脂羊毛中除虫脲和杀铃脲残留量进行准确的定性定量分析。

Simultaneous determination of diflubenzuron and triflumuron residues in greasy wool using high performance liquid chromatography

new method has been developed for the simultaneous determination of diflubenzuron and triflumuron residues in greasy wool by reversed-phase high performance liquid chromatography (HPLC). The pesticides were extracted by hexane-ether from greasy wool and cleaned up with gel permeation chromatography (GPC) and solid phase extraction (SPE). The pesticides were analyzed by HPLC-diode array detector (DAD) and quantified by external standard method. The linear ranges of diflubenzuron and triflumuron were 0.41-41 mg/L and 0.38-38 mg/L, and the correlation coefficients were 0.9996 and 0.9999, respectively. The limits of detection were 0.22 mg/kg for diflubenzuron and 0.18 mg/kg for triflumuron; the limits of quantification were 0.73 mg/kg for diflubenzuron and 0.60 mg/kg for triflumuron. The average recoveries of pesticides spiked levels from 0.76 to 10.25 mg/kg in greasy wool samples were in the range of 86.3%-96.7%, and the relative standard deviations were 4.2%-8.7%. The method developed shows little interferences, good recovery and repeatability. It is suitable for the simultaneous determination of diflubenzuron and triflumuron in greasy wool samples.