Wang Heng, Zhao Jie, Chen Zhiwei, He Pingang, Fang Yuzhi
Department of Chemistry, East China Normal University, Shanghai 200062, China.
Se Pu. 2008 Nov;26(6):740-3.
A 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 0.999 6 and 0.999 9, 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.
已开发出一种反相高效液相色谱法（HPLC）同时测定含脂羊毛中敌草隆和氟铃脲残留量的新方法。用正己烷 - 乙醚从含脂羊毛中提取农药，并用凝胶渗透色谱法（GPC）和固相萃取法（SPE）进行净化。通过HPLC - 二极管阵列检测器（DAD）分析农药，并采用外标法进行定量。敌草隆和氟铃脲的线性范围分别为0.41 - 41 mg/L和0.38 - 38 mg/L，相关系数分别为0.999 6和0.999 9。敌草隆的检测限为0.22 mg/kg，氟铃脲的检测限为0.18 mg/kg；敌草隆的定量限为0.73 mg/kg，氟铃脲的定量限为0.60 mg/kg。在含脂羊毛样品中添加0.76至10.25 mg/kg水平的农药，平均回收率在86.3% - 96.7%范围内，相对标准偏差为4.2% - 8.7%。所开发的方法干扰小、回收率好且重复性好。适用于同时测定含脂羊毛样品中的敌草隆和氟铃脲。
