基质固相分散-高效液相色谱法测定甘蔗中痕量甲拌磷和特丁硫磷

Matrix solid-phase dispersion and high performance liquid chromatography for the determination of phorate and terbufos in sugarcane

建立了基质固相分散(MSPD)-高效液相色谱紫外检测法(HPLC/UVD)测定甘蔗中痕量甲拌磷、特丁硫磷农药残留量的方法。甘蔗样品经弗罗里硅土研磨均匀后,石墨化碳黑净化,丙酮作为洗脱液,甲醇-水(体积比10:1)为流动相,HPLC/UVD进行分析检测。结果表明:在1.0～30.0μg/mL和1.0～40.0μg/mL范围内,甲拌磷和特丁硫磷浓度与峰面积呈良好的线性关系;样品加标平均回收率为82.6%～92.4%,相对标准偏差(RSD)为3.4%～6.7%。

The contents of phorate and terbufos in sugarcanes were studied by high performance liquid chromatography/ ultraviolet detector （HPLC/UVD） with matrix solid phase dispersion. The method which required Florisil as solid dispersion sorbent, graphitized carbon black as purificant and acetone as eluting solvent, was simple, fast and suitable for the preparation of a large number of sugarcanes samples. The samples were analyzed by HPLC/UVD with methanol-water （10：1,V/V） as mobile phase. The results showed that linear ranges of phorate and terbufos were 1.0-30.0μg/mL and 1.0-40.0μg/mL, respectively. The recoveries of spiked samples ranging from 82.6% to 92.4%, and relative standard deviations ranging from 3.4% to 6.7% were obtained.